# Dextroamphetamine synthesis (Nabenhower, 1942)



## G.Patton

*Introduction*​At the moment, there are many ways to synthesize dextroamphetamine. They can be divided into 3 types: biosynthesis (using biomass), direct synthesis, and synthesis of racemic (the sum of l- and d-isomers) amphetamine followed by separation of optical isomers. In our case, a synthesis was chosen, in which simple reagents and rapid synthesis were used, which is maximally adapted to «home conditions». The process is as follows: we obtain the racemic amphetamine in the classical way, then we divide it into 2 optical isomers (_l-_ and _d-_) by the Nabenhower method [US patent 2276508, Nabenhauer FP, "Method for the separation of optically active alpha-methylphenethylamine", published 17 March 1942, assigned to Smith Kline French].​*Synthesis*​Synthesis of amphetamine from P2NP via Al/Hg. First, we make an aluminum amalgam. It is needed in order to clean the aluminum from the strong oxide layer that forms when interacting with air. We take 14 g of aluminum foil and tear it with our hands into pieces of 2x2, 3x3 cm in size. Be sure to tear, not cut, to increase the surface area. Place into a 3-necked round-bottomed flask and fill the foil completely with water.​


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​Now we are preparing the mercury salt. We take a mercury thermometer from the pharmacy, wrap it in paper, break it at the bottom tip. Pour all the mercury into a glass, where then add 4 ml of nitric acid (70%). Do not forget that mercury vapors are hazardous to health! To initiate the reaction, the glass had to be heated to about 50 degrees, stirring occasionally. All the mercury dissolved about for 30 minutes, and an orange gas, nitrogen oxide (IV), was released from the glass. The reaction equation is as follows:​Hg + 4HNO3 ----> Hg(NO3)2 + 2NO2 + 2H2O


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​Pipette 2 ml of the solution and place it in a round-bottom flask with foil. After about 5 minutes, the foil lost its shine, became dull, and a small layer of gray sludge (aluminum hydroxide) collected at the bottom of the flask.​


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​We drain the liquid and rinse the foil with water 3 times.



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​Pour 30 ml of water into the flask, insert a thermometer into the left throat of the flask, insert a reflux condenser into the central throat, and insert a dropping funnel with 110 ml of 14% P2NP (it is phenylnitropropene; 1-phenyl-2-methyl-2-nitroethylene) solution into the right throat.​


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​Acetic essence is often used to produce hydrogen, but I "start" the reaction to produce hydrogen with water. Less acidic medium, which means less alkali must be added later. Many people ask the question: "How to remove this water?" There is no need to remove water anywhere, it reacts with aluminum and hydrogen is obtained:​2Al + 6H2O ---> 2Al (OH) 3 + 3H2​It is very important to remember that the reaction of P2NP reduction comes with a very! large exotherm. It is necessary to carefully monitor the temperature and prevent overheating above 60 degrees. Personally, I kept the temperature around 50-55 degrees. Failure to comply with this technology reduces the yield of the product and gives a colored (pink, orange) product. The infusion of the entire P2NP took about 50 minutes. Change the dropping funnel to a glass stopper. We got just such a gray solution.​


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​To increase the yield, you can heat the reaction mass at a temperature of 50-60 degrees for 30 minutes in a water bath.



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​We cool the mixture to room temperature, put a plug instead of the thermometer, remove the reflux condenser. We make an alkali solution based on 1 part of sodium hydroxide - 2 parts of water. Dissolution proceeds with heating, so we wait until the solution cools down. It is not worth pouring solid alkali into the reaction mass or pouring a hot solution, as this reduces the yield, like any overheating. Pour alkali cooled to room temperature to the reaction mass until pH = 11-12, wait 30-40 minutes until all the floating aluminum dissolves, yellow oil floats up. At the same time, we also monitor the temperature. Reaction equations:​*2Al + 2NaOH + 6H2O ==> 2Na[Al(OH4)] + 3H2
NaOH + Al (OH)3 ---> Na[Al(OH)4]*



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​We pour everything into a separating funnel. We are waiting for the separation of layers. Take the oily fraction.



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​We extract amphetamine from the sludge, washing it 3 times with 10 ml of petroleum ether. Divide the upper part with a separating funnel. Combine all extracts with "oil" and put them in ice water for cooling.



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​A large drop of water remains in the bottom of the glass, which is separated on a separating funnel. Pour the top layer into a glass and dry over anhydrous magnesium sulfate. There we clean the amphetamine from the remnants of mercury and water.​


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​We filter the liquid from solid magnesium sulfate on a Buchner funnel.



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​I take concentrated 98% sulfuric acid. Prepare a solution of sulfuric acid in acetone in a volume ratio of 1:10. I took the technical acetone, in the hardware store, and distilled it, taking away the "heads" and "tails". Then I dried it with anhydrous magnesium sulfate. Many people ask whether is it possible to make a solution in IPA. Yes, you can, but IPA (isopropyl alcohol) is evaporated longer than acetone.​


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​Drop by drop, carefully and with stirring, acidify with sulfuric acid in acetone to pH = 6. A white precipitate forms at the bottom.



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​Cool the reaction mass in ice water, filter the precipitate on a Buchner funnel, rinse with 3 ml of cold acetone.​


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​Air dry the filtered product and weight.



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​7.55 g (0.0205 mol) of amphetamine sulfate was obtained.
_Calculations:_
m (P2NP) = 110 * 0.14 = 15.4 g.
n (P2NP) = 15.4 / 163.17 = 0.094 mol.
n (amphetamine sulfate) = n (P2NP) = 0.094 mol.
n (amphetamine base)= 0.0205 * 2 = 0.0410 mol.
The reaction yield is 0.0410 /0.094 = 43.6 %.
You will carry out different reaction with sulfuric acid. Amphetamine free base 2 mole + 1 mole of sulfuric acid = 1 mole of amphetamine sulphate. When you count amph. sulphate, you have to multiply by two your mole result of amph. sulphate cuz you take 2 mole amph. base for one mole of amph sulfate.​*Extraction of d-amphetamine*​We've got racemic amphetamine. It contains 1 molecule of d-amphetamine per 1 molecule of l-amphetamine. Next, 6 g of racemate is taken and dissolved in 6 ml of water, an alkali solution is added to reach pH = 11.​


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​Extract with 5 ml of petroleum ether and warm the solution, add 2.45 g of d-tartaric acid in alcohol solution to the mixture. Then add alcohol until completely dissolved and cool with stirring. The l-amphetamine d-tartaric salt precipitates. The _d-amphetamine_ remains in the solution. You can repeat procedure of cleaning precipitate of l-amphetamine d-tartaric salt by methanol to increase yield.​


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​We precipitate d-amphetamine with an additional amount of d-tartaric acid. We filter the precipitate, get the base of d-amphetamine, adding alkali to pH = 11.



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​We acidify the d-amphetamine base to pH = 6 with a solution of sulfuric acid in acetone. This gives 2.63 g of d-amphetamine sulfate. Yield is 2.63 / 3 = 87.7%



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​This extraction method valid to amphetamine, which was synthesized by any routes. There is another way to obtain dextroamphetamine.


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## diogenes

Hi, great explanation, I have been looking for this clarity for a long time. Just two questions. Pure H2SO4 is difficult to optain in my country, they are selling aquarium Ph adjuster containing H3SO4 (Orthosulphuric acid), would this also be good. What is the best commercially available sulphate recommended by you? What should be used for basifying the solution (commercially available). I think caustic soda comes in lower concentration, would this also be suffice? thank you for your help


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## G.Patton

diogenes said:


> Hi, great explanation, I have been looking for this clarity for a long time. Just two questions. Pure H2SO4 is difficult to optain in my country, they are selling aquarium Ph adjuster containing H3SO4 (Orthosulphuric acid), would this also be good. What is the best commercially available sulphate recommended by you? What should be used for basifying the solution (commercially available). I think caustic soda comes in lower concentration, would this also be suffice? thank you for your help



diogenesHello. You can use diluted sulfuric acid (H2SO4), but in larger load. Sulfurous acid (H2SO3) isn't suitable because it's a weak acid and sulfuric acid (H2SO4) is strong. Caustic soda is the same as sodium hydroxide.
H3SO4 (Orthosulphuric acid) do not exist.


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## diogenes

Hi, sorry my bad I just stupidly confused Phosphoric acid (H3PO4) with Sulphuric acid (H2SO4). My question is basically where to get Sulphuric acid (H2SO4). Phosporic acid is easily available, but somehow I don`t find it as stimulating as the sulphate. (Your post finally clarifies and quantifies the difference an another topic, but even when adjusting for the dose it falls behind - I wonder whether absorption/excretion could be different - but this is off topic here.) So it would be great if I could try this separation method with D-sulphate in the end. 

Another question, does the type or concentration of alcohol matter when adding the tartaric acid? thank you


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## G.Patton

diogenes said:


> does the type or concentration of alcohol matter when adding the tartaric acid



diogenesNo matter.



diogenes said:


> where to get Sulphuric acid (H2SO4)


You can find it as accumulator electrolyte in hardware store or auto shop, it contains ~36% sulfuric acid


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## diogenes

Thank you for the information, it worked miraculously. I have evaporated the water and now have a pretty concentrated H2SO4. What is the proportion of sulphuric acid and aceton? Are they not going to make all kinds of new molecules when mixed together? Sorry if it is a dumb question but I`m a bit wary of mixing the two together. Also the NaOH solution for basifying: I have about 40% solution, does the concentration matter?


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## G.Patton

diogenes said:


> proportion of sulphuric acid and aceton?



diogenesPrepare a solution of sulfuric acid in acetone in a volume ratio of 1:10. (с)
Take 1 volume of acid and 10 volumes of acetone



diogenes said:


> I have about 40% solution, does the concentration matter?


It will be okay. You have to reach pH= 11-12, so, concentration not so important.


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## diogenes

Thank you very much Patton. I will report back when I try this separation, I hope I will get relatively good yields.


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## G.Patton

diogenes said:


> Thank you very much Patton. I will report back when I try this separation, I hope I will get relatively good yields.



diogenesGood luck, man!


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## diogenes

Hi again  I was looking at the numbers in the procedure as still waiting for some solvents to arrive. When starting the D-amphetamine purification, the 6ml of water given seems way too little. The solubility of the sulphate salt is given as 8.8 part water to one part amph. sulphate. Is it not a typo, did you not mean 60ml? Here is a link, but haven`t double-checked in the Merck:





Ask Erowid : ID 2057 : How does dissolving amphetamine in a liquid affect its potency?


Ask Erowid Question and Answer: How does dissolving amphetamine in a liquid affect its potency?



www.erowid.org





Reading the original patent, Nabenhauer seems to say that if deficient amount of D-Tartaric acid is added, then the L-isoform crystalises first (as described by you above), however, if D-tartaric acid is added in excess, then it is the D-isoform which crystalizes first. Can you, by any chance, explain the chemistry behind this? Why is one isomer quicker to crystalize than the other? Why does it change when excess tartaric acid is added?

I`d really appreciate if you could shed some light on this, I could not find a source, but perhaps this is because it is obvious for someone with more chemistry knowledge/experience. thank you


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## G.Patton

diogenes said:


> Hi again  I was looking at the numbers in the procedure as still waiting for some solvents to arrive. When starting the D-amphetamine purification, the 6ml of water given seems way too little. The solubility of the sulphate salt is given as 8.8 part water to one part amph. sulphate. Is it not a typo, did you not mean 60ml? Here is a link, but haven`t double-checked in the Merck:



diogenesYou can add water until it dissolves completely with minimum water. After, you'll add alkaline water solution with water, which will help to dissolve it as well.


diogenes said:


> Reading the original patent, Nabenhauer seems to say that if deficient amount of D-Tartaric acid is added, then the L-isoform crystalises first (as described by you above), however, if D-tartaric acid is added in excess, then it is the D-isoform which crystalizes first. Can you, by any chance, explain the chemistry behind this? Why is one isomer quicker to crystalize than the other? Why does it change when excess tartaric acid is added?
> 
> I`d really appreciate if you could shed some light on this, I could not find a source, but perhaps this is because it is obvious for someone with more chemistry knowledge/experience. thank you


Simply say: firstly, stereoselective reaction is carried out on more "easier" and low-energy way with l-isomer and after goes by second way on more high-energy way.


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## SergMarsian

G.Patton said:


> ​We precipitate d-amphetamine with an additional amount of d-tartaric acid. We filter the precipitate, get the base of d-amphetamine, adding alkali to pH = 11.
> ​We acidify the d-amphetamine base to pH = 6 with a solution of sulfuric acid in acetone. This gives 2.63 g of d-amphetamine sulfate. Yield 2.63 / 3 = 87.7%
> ​This extraction method valid to amphetamine, which was synthesized by any routes. There is another way to obtain dextroamphetamine.



G.PattonHello, since there is no dextroamphetamine on the market and I need it, there is a need to make it for myself on my own, I am a beginner, so I have some questions, as I understand it first with the use of tartaric acid with methanol - L amphetamine falls into the precipitate and then you need to take a solution without this precipitate and add without alcohol just d tartaric acid and add alkali until the PH reaches 11 and only then it can be filtered and get a dry base of D amphetamine, after which acidification with sulfuric acid in acetone and filtration to get dry pure d amphetamine, right?

Do need tartaric acid D(-) or D(+) ?


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## G.Patton

SergMarsian said:


> Do need tartaric acid D(-) or D(+) ?



SergMarsianHi, no difference.


SergMarsian said:


> with methanol


better to take ethanol


SergMarsian said:


> add without alcohol just d tartaric acid


"an additional amount of d-tartaric acid." Means d-tartaric acid alcohol solution, sorry for the inaccuracy.


SergMarsian said:


> add alkali until the PH reaches 11 and only then it can be filtered and get a dry base of D amphetamine, after which acidification with sulfuric acid in acetone and filtration to get dry pure d amphetamine, right?


affirmative


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## SergMarsian

G.Patton said:


> better to take ethanol
> 
> "an additional amount of d-tartaric acid." Means d-tartaric acid alcohol solution, sorry for the inaccuracy.



G.PattonThank you very much for the answers, another question about the alcoholic solution of d-tartaric acid, d tartaric acid with ethanol (96%) in what proportion to interfere? until the tartaric acid dissolves?


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## G.Patton

SergMarsian said:


> Thank you very much for the answers, another question about the alcoholic solution of d-tartaric acid, d tartaric acid with ethanol (96%) in what proportion to interfere? until the tartaric acid dissolves?



SergMarsianYou need pour minimum amount of alcohol to dissolve it


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## diogenes

SergMarsian said:


> and add alkali until the PH reaches 11 and only then it can be filtered and get a dry base of D amphetamine



SergMarsianHi Serg, I think it precipitates when you add the extra D-tartaric acid solution, and this is when you filter, so you get a more or less dry precipitate which is D-tartaric-D-amphetamine. Then you add some alkaline solution to free the base from the tartaric acid, so you get a thin film of D-amphetamine base on top of a water solution of Sodium and tartarate. Then you have to extract the base with as little solvent as possible to make it very dense, and then add Sulphuric acid/Acetone to this to precipitate D-amphetamine sulphate.


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## diogenes

SergMarsian said:


> Thank you very much for the answers, another question about the alcoholic solution of d-tartaric acid, d tartaric acid with ethanol (96%) in what proportion to interfere? until the tartaric acid dissolves?



SergMarsianPatton, would it not be better to use 100% ethanol, drying over some MgSO4 and distilling it?

Serg, we are pretty much in the same boat, I got into chemistry facing the same problem that only racemic amphetamine is available. That said, Patton makes it sound so easy, because it is easy once you are on his level in chemistry. There are many fine details you have to get right, e.g. having pure reagents anhydrous acetone, sulphuric acid etc.ILet me know how you get on.


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## G.Patton

diogenes said:


> Patton, would it not be better to use 100% ethanol, drying over some MgSO4 and distilling it?



diogenesYes, it's better to increase rxn yield


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## ASheSChem

G.Patton said:


> we take 6 g of racemate



G.Patton


G.Patton said:


> This gives 2.63 g of d-amphetamine sulfate. Yield 2.63 / 3 = 87.7%



i don't understand how you calculate yielding :x


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## G.Patton

ASheSChem said:


> i don't understand how you calculate yielding :x



ASheSChemWe took 6g of racemate = 3 g of D-amph+3 g of L-amph
We got
2.63g yield = x%
3.0g theory = 100%

2.63*100/3=87.7%


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## ASheSChem

hooo yes ok , thanks
possible to save the L-amph part?


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## dark_side_of_chemistry

I read the original patent. there they wrote that per 2mol of amphetamine they add 1mol of tartaric acid and dissolve it in the right amount of alcohol. heat to a boil and set aside to crystallize. they separate the aqueous phase from the crystals and carry out another recrystallization. they repeat this operation several times. then alkali is added to the combined water phases to raise the pH to 11. two phases are formed. one is oil. I understood the original patent well. will the actions carried out in this way give the appropriate effect?https://patents.google.com/patent/US2276508A/en
Two mols, for example, 2'70 grams, of racemic e-methylphenethylamine base are reacted with one mol (1'50 grams) of d-tartaric acid, thereby forming d1-a-methylphenethylamine d-tartrate. a neutral salt. The neutral salt thus obtained is fully dissolved by the addition of sufficient, say about one liter, of absolute ethanol, and heating to about the boiling point. The solution is then allowed towel to room temperature with occasional stirring to eiiect crystallization. The crystals are filtered oil and will be found to contain a preponderance of the laevo enantiomorph. On recrystallization the preponderance of the lenantiomorph is increased and the process is repeated until no further change in optical rotation is effected and a reading of is obtained in a concentration of 8 grams per 100 cc. of aqueous solution. The product thus obtained is Liz-methylphenethylamine d-tartrate. The residual solid in the mother liquors is repeatedly and systematically crystallized, yielding a further fraction of biz-methylphenethylamine d-tartrate which may be purified by recrystallization. d-a-methylphenethylamine may be readily recovered from the mother liquors by the addition of tartaric acid thereto for the formation of acid tartrates and separation of d-a-methylphenethylamine d-bitartrate by crystallization. 
The free base'of either optical isomer may be obtained by addition to the d-tartrate in the case of the laevo isomer and the d-bitartrate in the case of the dextro isomer of alkali in excess, as, for example, by the addition of an aqueous solution of caustic soda, which will cause the base to separate as an oil which may be recovered and purified by any well known procedure.


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## diogenes

Hi, I need some help! I have tried the Rusznak method for resolving racemic amphetamine. Here is the only information from Erowid, I tried to search for the paper, but could not find anything:

_A mixture of 0.1 mole (13.52 g.) phenylisopropylamine (or 14.92 g. methamphetamine base) in 60 ml benzene, 0.05 mole d-tartaric acid (7.50 g.) in 30 ml water, and 2 g sodium hydroxide (reagent grade or titrated equivalent) in 3 ml water was kept 4 hours with intermittent shaking, and the organic phase evaporated to give 98% L-phenylisopropylamine. The aqueous phase was extracted with benzene at pH 13 and evaporated to give 96% D-enantiomer._​
I used half amounts compared to the description. Everything went fine, I got the Amphetamine disolved then base extracted with 30ml of *Toluene* (I didn`t have benzene - could this be the problem?), then added the other ingredients and kept for about 4 hours. There was some precipitate forming, but nothing some shaking in the separatory funnel would not help. Aqueous phase separated, and alkali given to PH 13. A nice layer of base formed on top of the water, so at this point I thought everything is fine. The base was extracted with 30ml of Toluene, however, when the acetone-sulphuric acid was added there was only a moderate precipitation, which did not increase, rather it started to disappear when a small layer of sulphuric acid - water was formed at the bottom of the beaker.

How can I save the hopefully D-Amphetamine extracted? I have also saved all the phases, so if someone points out a blunder earlier on, I can reverse. This is a very nice and easy method and I think it went fine, I just probably made some horrible mistakes in the simple extraction at the end. Actually wanted to re-read Patton`s extraction topic before starting with the final extraction, but was too excited and just went for it.
Any herlp would be appreciated.

My tips are:
- my acetone was not anhydrous - I distilled the acetone on NaSO4 yesterday and it was kept in a closed flask, but not in the freezer
- sulphuric acid contained water (it is pretty concentrated but not sure exactly - between 90-95%)
- I should have dried the Toluene before adding the acid - or perhaps just evaporate it a bit?
- Toluene is not the right solvent for this extraction for some reason (unknown to me).
- Should I reverse buy adding some alkali, then drying the Toluene, then let it evaporate?


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## diogenes

I have just realized that I omitted the last instruction which may be the solution to the problem. 

_The aqueous phase was extracted with benzene at pH 13 *and evaporated *to give 96% D-enantiomer._​
Still, even if evaporation works, what is the next thing to do to obtain D-Amphetamine sulphate? Just simply precipitate (acetone - sulphuric acid) but after evaporation? Why does it need to be evaporated? Is the reason that Toluene does not mix with Sulphuric acid, unlike IPA?


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## G.Patton

ASheSChem said:


> possible to save the L-amph part?



ASheSChemYes, you can filter L-amph D-tartaric acid after precipitation. *Why are you reinventing the wheel? *The method in this topic.


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## ASheSChem

sorry ;maybe i read too much for my little brain 
you clearly explain it in the method.. 

Thanks for your works !


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## diogenes

Hi Patton, when you used 6g of the Amphetamine sulphate in the above extraction and then added half of the amount of D-Tartaric acid (in terms of mol). I think 3.3g is too much because when calculating the molar amount the freebase needs to be taken into account. 6g of Amphetamine sulphate is 4.4g freebase, which is 0.0326 Mol of base (1 Mol is 135g). We need 0.0326/2 Mol D-Tartaric acid which is roughly *2.446g*. Let me know if my thinking is on the right track. If yes, then it is thanks to you for your Amphetamine salt topic. I was trying this extraction and tried to calculate how much L-Amphetamine-D-Tartaric acid precipitate I should get. 

By the way first I got way too little precipitate, just above 1g after drying. I guess this is why the author of the patent says to continue the crystalisation until we get a solution with the right rotation? I`m thinking of trying to put the solution into the freezer so that more L-Amphetamine-D-Tartaric acid can precipitate? It would be much more comfortable not having to do the crystallisation so many times.


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## G.Patton

diogenes said:


> Hi Patton, when you used 6g of the Amphetamine sulphate in the above extraction and then added half of the amount of D-Tartaric acid (in terms of mol). I think 3.3g is too much because when calculating the molar amount the freebase needs to be taken into account. 6g of Amphetamine sulphate is 4.4g freebase, which is 0.0326 Mol of base (1 Mol is 135g). We need 0.0326/2 Mol D-Tartaric acid which is roughly *2.446g*. Let me know if my thinking is on the right track. If yes, then it is thanks to you for your Amphetamine salt topic. I was trying this extraction and tried to calculate how much L-Amphetamine-D-Tartaric acid precipitate I should get.



diogenesYou absolutely right. I'll fix my mistake.


diogenes said:


> By the way first I got way too little precipitate, just above 1g after drying. I guess this is why the author of the patent says to continue the crystalisation until we get a solution with the right rotation? I`m thinking of trying to put the solution into the freezer so that more L-Amphetamine-D-Tartaric acid can precipitate? It would be much more comfortable not having to do the crystallisation so many times.


Let us know your result, please.


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## Heartburn

I've got two questions.
What to do with L-amph tartrate, since it's main effects are not very desirable for user? 
What is the maximum shelf time of tartrate salts in comparison with sulphate/phosphate?


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## G.Patton

Heartburn said:


> What to do with L-amph tartrate, since it's main effects are not very desirable for user?



HeartburnEffects weaker than d-amph sulphate.


Heartburn said:


> What is the maximum shelf time of tartrate salts in comparison with sulphate/phosphate?


I can't say exactly, I think the same.


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## diogenes

Heartburn said:


> I've got two questions.
> What to do with L-amph tartrate, since it's main effects are not very desirable for user?
> What is the maximum shelf time of tartrate salts in comparison with sulphate/phosphate?



HeartburnI would simply discard of L-amphetamine tartarate otherwise what is the point of separation?
I think tartarate salts are rather hydrophilic, they absorb water so storing them becomes more problematic, just like Amphetamine-HCL. This is why sulphate/phosphate salts are more desirable.


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## Joker_333

G.Patton said:


> *Introduction*​At the moment, there are many ways to synthesize dextroamphetamine. They can be divided into 3 types: biosynthesis (using biomass), direct synthesis, and synthesis of racemic (the sum of l- and d-isomers) amphetamine followed by separation of optical isomers. In our case, a synthesis was chosen, in which simple reagents and rapid synthesis were used, which is maximally adapted to «home conditions». The process is as follows: we obtain the racemic amphetamine in the classical way, then we divide it into 2 optical isomers (_l-_ and _d-_) by the Nabenhower method [US patent 2276508, Nabenhauer FP, "Method for the separation of optically active alpha-methylphenethylamine", published 17 March 1942, assigned to Smith Kline French].​*Synthesis*​Synthesis of amphetamine from P2NP via Al/Hg. First, we make an aluminum amalgam. It is needed in order to clean the aluminum from the strong oxide layer that forms when interacting with air. We take 14 g of aluminum foil and tear it with our hands into pieces of 2x2, 3x3 cm in size. Be sure to tear, not cut, to increase the surface area. Place into a 3-necked round-bottomed flask and fill the foil completely with water.​
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> Now we are preparing the mercury salt. We take a mercury thermometer from the pharmacy, wrap it in paper, break it at the bottom tip. Pour all the mercury into a glass, where then add 4 ml of nitric acid (70%). Do not forget that mercury vapors are hazardous to health! To initiate the reaction, the glass had to be heated to about 50 degrees, stirring occasionally. All the mercury dissolved about for 30 minutes, and an orange gas, nitrogen oxide (IV), was released from the glass. The reaction equation is as follows:​Hg + 4HNO3 ----> Hg(NO3)2 + 2NO2 + 2H2O
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> Pipette 2 ml of the solution and place it in a round-bottom flask with foil. After about 5 minutes, the foil lost its shine, became dull, and a small layer of gray sludge (aluminum hydroxide) collected at the bottom of the flask.​
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> We drain the liquid and rinse the foil with water 3 times.
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> Pour 30 ml of water into the flask, insert a thermometer into the left throat of the flask, insert a reflux condenser into the central throat, and insert a dropping funnel with 110 ml of 14% P2NP (it is phenylnitropropene; 1-phenyl-2-methyl-2-nitroethylene) solution into the right throat.​
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> Acetic essence is often used to produce hydrogen, but I "start" the reaction to produce hydrogen with water. Less acidic medium, which means less alkali must be added later. Many people ask the question: "How to remove this water?" There is no need to remove water anywhere, it reacts with aluminum and hydrogen is obtained:​2Al + 6H2O ---> 2Al (OH) 3 + 3H2​It is very important to remember that the reaction of P2NP reduction comes with a very! large exotherm. It is necessary to carefully monitor the temperature and prevent overheating above 60 degrees. Personally, I kept the temperature around 50-55 degrees. Failure to comply with this technology reduces the yield of the product and gives a colored (pink, orange) product. The infusion of the entire P2NP took about 50 minutes. Change the dropping funnel to a glass stopper. We got just such a gray solution.​
> 
> Spoiler: Pic.6
> 
> 
> 
> View attachment 3167
> 
> 
> To increase the yield, you can heat the reaction mass at a temperature of 50-60 degrees for 30 minutes in a water bath.
> 
> 
> Spoiler: Pic.7
> 
> 
> 
> View attachment 1454
> 
> 
> We cool the mixture to room temperature, put a plug instead of the thermometer, remove the reflux condenser. We make an alkali solution based on 1 part of sodium hydroxide - 2 parts of water. Dissolution proceeds with heating, so we wait until the solution cools down. It is not worth pouring solid alkali into the reaction mass or pouring a hot solution, as this reduces the yield, like any overheating. Pour alkali cooled to room temperature to the reaction mass until pH = 11-12, wait 30-40 minutes until all the floating aluminum dissolves, yellow oil floats up. At the same time, we also monitor the temperature. Reaction equations:​6NaOH + 2Al + 6H2O ---> 2Na3 [Al (OH) 6] + 3H2
> 3NaOH + Al (OH) 3 ---> Na3 [Al (OH) 6]
> 
> 
> Spoiler: Pic.8
> 
> 
> 
> View attachment 3168
> 
> 
> We pour everything into a separating funnel. We are waiting for the separation of layers. Take the oily fraction.
> 
> 
> Spoiler: Pic.9
> 
> 
> 
> View attachment 3169
> 
> 
> We extract amphetamine from the sludge, washing it 3 times with 10 ml of petroleum ether. Divide the upper part with a separating funnel. Combine all extracts with "oil" and put them in ice water for cooling.
> 
> 
> Spoiler: Pic.10
> 
> 
> 
> View attachment 1457
> 
> 
> A large drop of water remains in the bottom of the glass, which is separated on a separating funnel. Pour the top layer into a glass and dry over anhydrous magnesium sulfate. There we clean the amphetamine from the remnants of mercury and water.​
> 
> Spoiler: Pic.11
> 
> 
> 
> View attachment 1458
> 
> 
> We filter the liquid from solid magnesium sulfate on a Buchner funnel.
> 
> 
> Spoiler: Pic.12
> 
> 
> 
> View attachment 3170
> 
> 
> I take concentrated 98% sulfuric acid. Prepare a solution of sulfuric acid in acetone in a volume ratio of 1:10. I took the technical acetone, in the hardware store, and distilled it, taking away the "heads" and "tails". Then I dried it with anhydrous magnesium sulfate. Many people ask whether it is possible to make a solution in IPA. Yes, you can, but IPA (isopropyl alcohol) dries longer than acetone.​
> 
> Spoiler: Pic.13
> 
> 
> 
> View attachment 3171
> 
> 
> Drop by drop, carefully and with stirring, acidify with sulfuric acid in acetone to pH = 6. A white precipitate forms at the bottom.
> 
> 
> Spoiler: Pic.14
> 
> 
> 
> View attachment 1461
> 
> 
> Cool the reaction mass in ice water, filter the precipitate on a Buchner funnel, rinse with 3 ml of cold acetone.​
> 
> Spoiler: Pic.15
> 
> 
> 
> View attachment 3172
> 
> 
> Air dry the filtered product and weight.
> 
> 
> Spoiler: Pic.16
> 
> 
> 
> View attachment 1464
> 
> 
> 7.55 g (0.0205 mol) of amphetamine sulfate was obtained.
> _Calculations:_
> m (P2NP) = 110 * 0.14 = 15.4 g.
> n (P2NP) = 15.4 / 163.17 = 0.094 mol.
> n (amphetamine sulfate) = n (P2NP) = 0.094 mol.
> n (amphetamine base)= 0.0205 * 2 = 0.0410 mol.
> The reaction yield is 0.0410 /0.094 = 43.6 %.
> You will carry out different reaction with sulfuric acid. Amphetamine free base 2 mole + 1 mole of sulfuric acid = 1 mole of amphetamine sulphate. When you count amph. sulphate, you have to multiply by two your mole result of amph. sulphate cuz you take 2 mole amph. base for one mole of amph sulfate.​*Extraction of d-amphetamine*​We've got racemic amphetamine. It contains 1 molecule of d-amphetamine per 1 molecule of l-amphetamine. Next, we take 6 g of racemate and dissolve in 6 ml of water, add an alkali solution to pH = 11.​
> 
> Spoiler: Pic.17
> 
> 
> 
> View attachment 1466
> 
> 
> Extract with 5 ml of petroleum ether and warm the solution, add 2.45 g of d-tartaric acid in alcohol solution to the mixture. Then add alcohol until completely dissolved and cool with stirring. The l-amphetamine d-tartaric salt precipitates. The _d-amphetamine_ remains in the solution. You can repeat procedure of cleaning precipitate of l-amphetamine d-tartaric salt by methanol to increase yield.​
> 
> Spoiler: Pic.18
> 
> 
> 
> View attachment 3173
> 
> 
> We precipitate d-amphetamine with an additional amount of d-tartaric acid. We filter the precipitate, get the base of d-amphetamine, adding alkali to pH = 11.
> 
> 
> Spoiler: Pic.19
> 
> 
> 
> View attachment 1470
> 
> 
> We acidify the d-amphetamine base to pH = 6 with a solution of sulfuric acid in acetone. This gives 2.63 g of d-amphetamine sulfate. Yield 2.63 / 3 = 87.7%
> 
> 
> Spoiler: Pic.20
> 
> 
> 
> View attachment 1471
> 
> 
> This extraction method valid to amphetamine, which was synthesized by any routes. There is another way to obtain dextroamphetamine.



G.PattonHi Can mercury chloride be used instead of mercury nitrate?


----------



## T0R

Joker_333 said:


> Hi Can mercury chloride be used instead of mercury nitrate?



Joker_333
yes


----------



## UWe9o12jkied91d

Joker_333 said:


> Hi Can mercury chloride be used instead of mercury nitrate?



Joker_333(II), (I) will not work


----------



## SpeeD

P2NP 14% in Nitroethane, correct? ​G.Patton​


----------



## UWe9o12jkied91d

It's in isopropanol using nitroethane here as a solvent would be 1 stupid 2 wasteful


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## G.Patton

SpeeD said:


> in Nitroethane



SpeeDIn IPA


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## UWe9o12jkied91d

diogenes said:


> I would simply discard of L-amphetamine tartarate otherwise what is the point of separation?
> I think tartarate salts are rather hydrophilic, they absorb water so storing them becomes more problematic, just like Amphetamine-HCL. This is why sulphate/phosphate salts are more desirable.



diogenesYou can racemize the 50% lisomer you are left with and repeat as many times as possible.You do 3 of them bam 90% ish theoretical yield of the wanted isomer.


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## diogenes

UWe9o12jkied91d said:


> You can racemize the 50% lisomer you are left with and repeat as many times as possible.You do 3 of them bam 90% ish theoretical yield of the wanted isomer.



UWe9o12jkied91dHow do you racemize it? I haven`t heard about such method.


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## UWe9o12jkied91d

diogenes said:


> How do you racemize it? I haven`t heard about such method.



diogenesHere you go, good sir, from the horse's mouth.Kind of dangerous to have the stuff laying around, so probably not worth it for the chemist producing for himself.This article talks about methyl-amp. but I am 100% sure you can do this with the unmethylated variant.



https://www.emcdda.europa.eu/publications/eu-drug-markets/methamphetamine/main-production-methods-europe_en#figure7


[/URL]


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## wannabeechemist

G.Patton​Sulfate isn't perfectly white. You got rid of all water soluble impurities, now that's left to do few washings with acetone/IPA and should be left with ~95% pure salt?

I guess in that case there is no need to steam distill, no?

I ask because my gear is textbook looking but is active at high dosages and the high feels somewhat dirty.


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## G.Patton

wannabeechemist said:


> Sulfate isn't perfectly white.



wannabeechemistIt is. I got absolutely white powder and saw different ones with good quality. Sometimes it has a little tint.


wannabeechemist said:


> now that's left to do few washings with acetone/IPA and should be left with ~95% pure salt?


Yes, should be. Some amphetamine-relaed by-products still will be there. Steam distillation is a good option to get rid of by-products with different boiling point (for amph free base).


----------



## johski

3 quick questions, not all on topic here... wash meth with dichloromethane first? good or bad idea? what is the best way to make the freebase? Can the above procedures for amphetamine apply/take over methamphetamine as well?


----------



## G.Patton

johski said:


> 3 quick questions, not all on topic here... wash meth with dichloromethane first? good or bad idea? what is the best way to make the freebase? Can the above procedures for amphetamine apply/take over methamphetamine as well?



johskiYou can open Meth topics and read/ask there.


johski said:


> Can the above procedures for amphetamine apply/take over methamphetamine as well?





http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/synthesis-of-methamphetamine-from-p2p-via-aluminum-amalgam.184/




http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/methamphetamine-from-p2p-by-nabh4-reduction-medium-scale.600/


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## MadHatter

I'll put this here also:
What really messed with my head in this description was the nomenclature concerning the tartaric acid. The text in the description uses the old nomenclature for the tartaric acid isomers, with lowercase "d" for dextro-tartaric acid. In modern texts and when you buy tartaric acid a capital "L" will be used for the same isomer: L-tartaric acid. So "d-tartaric acid" is the same thing as "L-tartaric acid".

To confuse things further, the other isomer, Levo-tartaric acid, is named "l-tartaric acid" in older texts, but "D-tartaric acid" in modern texts and in chemical companies. 

Now, *D-tartaric acid* (formerly _l-tartaric acid_) is really expensive and difficult to buy. Often times it requires an End User Declaration to purchase in larger quantities. 
*L-tartaric acid* (formerly _d-tartaric acid_) is however both cheap and accessible. It's a natural acid derived from fruits and available to buy from winemaking stores online. This is the one you want. 
it's also very usable to resolve (it's called _resolving_ when you separate enantiomers) methamphetamine, which is even more crucial since the L-isomer of meth is useless. 

There's a pretty good article about resolving amphetamine isomers here, called "The Dutch Solution": (WARNING clearnet) https://www.thevespiary.org/rhodium/Rhodium/chemistry/amphetamine.resolution.html

This is an excerpt from the text concerning the separation of meth isomers:

_Resolution of racemic Methamphetamine_​_85 parts of racemic methamphetamine are introduced into a solution of 100 parts of d-tartaric acid in 1000 parts of methyl alcohol. After protracted standing about 100 parts of the precipitated salt are aspirated off and extracted with hot ethyl alcohol. Since the d-tartrate of dextrorotary methamphetamine is readily soluble in both methyl and ethyl alcohol whereas the d-tartrate of levorotary methamphetamine is sparingly soluble both in methyl alcohol and hot ethyl alcohol an extremely simple separation of the d-tartrates of the optical antipodes of the base is effected.

*Reference:* British Patent 508,757_

So basically you dissolve meth or amph freebase in near-boiling methanol with L-tartaric acid in. Once the solution cools, crystals of l-amph/l-meth bound to L-tartaric acid will begin to crash out. You just filter these out and discard or save them. 
I would then basify the solution with NaOH and evaporate off much off the alcohol, and add water to get a good separation of the freebase layer, extract it in a sep funnel and then bubble HCl gas through it if it's d-meth freebase or add sulphuric acid if it's d-amph freebase to get nice d-crystals.


----------



## G.Patton

DocX said:


> So "d-tartaric acid" is the same thing as "L-tartaric acid".



DocXHi, you are *wrong*. They are *different* isomers. Please, read about isomers of Tartaric acid here.


----------



## MadHatter

G.Patton said:


> Hi, you are *wrong*. They are *different* isomers. Please, read about isomers of Tartaric acid here.
> View attachment 6601​



G.PattonFrom the wikipedia article you just linked to:

___________________________
Naturally occurring form of the acid is *dextro tartaric acid *or *L-(+)-tartaric acid* (obsolete name _d_-tartaric acid). Because it is available naturally, it is cheaper than its enantiomer and the meso isomer. The _dextro_ and _levo_ prefixes are archaic terms.[13] Modern textbooks refer to the natural form as (2_R_,3_R_)-tartaric acid *(*L*-(+)-tartaric acid)*, and its enantiomer as (2_S_,3_S_)-tartaric acid *(*D*-(-)-tartaric acid)*. The _meso_ diastereomer is referred to as (2_R_,3_S_)-tartaric acid or (2_S_,3_R_)-tartaric acid.
___________________________

Which is the opposite of what you just posted? And exactly what I wrote? This image is from the same wikipedia article:


----------



## MadHatter

So *L-(+)-tartaric acid* is the same thing as *d-tartaric acid* and *(2R,3R)-tartaric acid* which is *dextro* tartaric acid.
*D-(-)-tartaric acid* is the same thing as *l-tartaric acid* and *(2S,3S)-tartaric acid *which is _*levo*_ tartaric acid.

And *DL-tartaric acid* would be useless for resolution. Since it's a racemat itself and would crystallize both isomers of the amphetamine. 

Goddamn chemical nomenclature is a bad trip in itself.


----------



## G.Patton

DocX said:


> *dextro tartaric acid *or *L-(+)-tartaric acid* (obsolete name _d_-tartaric acid).



DocXI didn't read carefully. Actually it is not. I think there is mistake in Wiki because this statement contradicts to this picture. I've sent this pic which is clearly show that these are different isomers. I understand that it is hard to realize but...


----------



## MadHatter

Sorry for spamming, but I found the key. The image you post is from the wikipedia article on stereochemistry. It's faulty. That article is pretty heavily critizised in the Talk-section.

*The picture I post is the correct one. *

The prefixes *l* and *d* are just short for *dextrorotary* or *levorotary*: which way the molecule rotates polarized light. "*l*" = l*evo* = *to the left*, "*d*" = *dextro* = *to the right*. But these prefixes are old and not used anymore.
In the modern nomenclature these have been replaced by the *(+) *for _dextro_ and the *(-) *for _levo_.

The prefixes *L* and *D* _(uppercase letters)_ refer to the *Fischer projections* of the molecules and have nothing to do with how they rotate light, but in what direction key parts of the molecule is drawn. They are in this case actually _*REVERSED*_ in relation to the *d* and *l *prefixes: *d is L and l is D.*

So *L-(+)-tartaric acid* means: "_a tartaric acid molecule that's drawn with the highest priority group at the top on the Fischer projection and the relevant group pointed to the *L*eft, and rotates polarized light to the *right*_", a.k.a *dextrorotary*, a.k.a *dextro*, a.k.a *d-tartaric acid*. This is the natural form of tartaric acid.

And, of course, vice versa for *D-(-)-tartaric acid*.

Now, as far as I understand, both isomers of tartaric acid can be used to resolve enantiomers of amphetamines. If you use *D-(-)-tartaric acid* you will get crystals of *d-amph/D-tartrate* crashing out, and if you use *L-(+)-tartaric acid *you will get crystals of *l-amph/L-tartrate* crashing out.
Using *DL-tartaric acid* would be absolutely useless, since it wouldn't separate anything: both enantiomers would crash out.

Phew. 
I have spoken.


----------



## G.Patton

DocX said:


> Sorry for spamming, but I found the key. The image you post is from the wikipedia article on stereochemistry. It's faulty. That article is pretty heavily critizised in the Talk-section.
> 
> *The picture I post is the correct one. *
> 
> The prefixes *l* and *d* are just short for *dextrorotary* or *levorotary*: which way the molecule rotates polarized light. "*l*" = l*evo* = *to the left*, "*d*" = *dextro* = *to the right*. But these prefixes are old and not used anymore.
> In the modern nomenclature these have been replaced by the *(+) *for _dextro_ and the *(-) *for _levo_.
> 
> The prefixes *L* and *D* _(uppercase letters)_ refer to the *Fischer projections* of the molecules and have nothing to do with how they rotate light, but in what direction key parts of the molecule is drawn. They are in this case actually _*REVERSED*_ in relation to the *d* and *l *prefixes: *d is L and l is D.*
> 
> So *L-(+)-tartaric acid* means: "_a tartaric acid molecule that's drawn with the highest priority group at the top on the Fischer projection and rotates polarized light to the right_", a.k.a *dextrorotary*, a.k.a *dextro*, a.k.a *d-tartaric acid*. This is the natural form of tartaric acid.
> 
> And, of course, vice versa for *D-(-)-tartaric acid*.
> 
> Now, as far as I understand, both isomers of tartaric acid can be used to resolve enantiomers of amphetamines. If you use *D-(-)-tartaric acid* you will get crystals of *d-amph/D-tartrate* crashing out, and if you use *L-(+)-tartaric acid *you will get crystals of *l-amph/L-tartrate* crashing out.
> Using *DL-tartaric acid* would be absolutely useless, since it wouldn't separate anything: both enantiomers would crash out.
> 
> Phew. I have spoken.



DocXSorry, I was confused. L(+) isomer can be used to get (-)D-amph/methamph. Procedure a little bit different from mine and you can get another isomer. I worked with D-Isomer only. *You'll get D-amph L-tartaric acid as an precipitate.*


> Extract with 5 ml of petroleum ether and warm the solution, add 2.45 g of d-tartaric acid in alcohol solution to the mixture. Then add alcohol until completely dissolved and cool with stirring. The l-amphetamine d-tartaric salt precipitates. The _d-amphetamine_ remains in the solution. You can repeat procedure of cleaning precipitate of l-amphetamine d-tartaric salt by methanol to increase yield.


----------



## Mr.Blanks00

DocX said:


> So *L-(+)-tartaric acid* is the same thing as *d-tartaric acid* and *(2R,3R)-tartaric acid* which is *dextro* tartaric acid.
> *D-(-)-tartaric acid* is the same thing as *l-tartaric acid* and *(2S,3S)-tartaric acid *which is _*levo*_ tartaric acid.
> 
> And *DL-tartaric acid* would be useless for resolution. Since it's a racemat itself and would crystallize both isomers of the amphetamine.
> 
> Goddamn chemical nomenclature is a bad trip in itself.



DocXhi, is this product the same as L- and can it be used?


----------



## T0R

Yusuf said:


> hi, is this product the same as L- and can it be used?



Yusuf
search on the lable for the cas nr

D-Tartaric Acid CAS 147-71-7, 
L-Tartaric Acid CAS 87-69-4,

(1) dextrorotatory tartaric acid (d-tartaric acid) found in grapes and several other fruits,

(2) levorotatory tartaric acid (l-tartaric acid) obtained chiefly by resolution of racemic tartaric acid,


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## G.Patton

Yusuf said:


> hi, is this product the same as L- and can it be used?



Yusufread my previous message please


----------



## MadHatter

Yusuf said:


> hi, is this product the same as L- and can it be used?



YusufYes. Absolutely. It's *L-(+)-tartaric acid*, or *dextro tartaric acid*.
This is the same as *d-tartaric acid*.

Procedure: as in the description of this thread (for amphetamine) or as in *this* article (clearnet).


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## G.Patton

DocX said:


> Procedure: as in the description of this thread (for amphetamine) or as in *this* article (clearnet).



DocXWhy do you refer side resources while in this thread this procedure is described?


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## MadHatter

G.Patton said:


> Why do you refer side resources while in this thread this procedure is described?



G.PattonI _did_ refer to the description in the thread. Read the answer again. 

The other reference is broader and also gives information about the recrystallization of meth and how to use other resolving agents than the pure L-(+)-tartaric acid. I think it adds value to the thread. Surely it's ok to give references when you post info on this forum? At least, it has been done many times before. If you have issue with that reference, please tell what it is.


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## G.Patton

DocX said:


> other resolving agents than the pure L-(+)-tartaric acid.



DocXI didn't find any other option in this article. Also, recrystallization procedure is the same as for usual meth. By the way, you can use flash chromatography to separate isomers but this method to much complicated.


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## MadHatter

G.Patton said:


> I didn't find any other option in this article. Also, recrystallization procedure is the same as for usual meth. By the way, you can use flash chromatography to separate isomers but this method to much complicated.



G.PattonHaha, sorry! I thought I pasted the link to a Rhodium article . I'll fix my error.


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## MadHatter

This is the article I meant to reference: https://www.thevespiary.org/rhodium/Rhodium/chemistry/amphetamine.resolution.html

In that reference, they used this and seem to have made an analysis of the optical isomers isolated:




> Resolution of racemic Methamphetamine using O,O-Dibenzoyl-R,R-Tartaric Acid​Using O,O-Dibenzoyl-2R,3R-Tartaric Acid (made by acylating L(+)-tartaric acid with benzoyl chloride) in dichloroethane/methanol/water, racemic methamphetamine can be resolved in 80-95% yield, with an optical purity of 85-98%.
> 
> *Experimental*
> 
> 15.0g (100 mmol) of racemic methamphetamine freebase was dissolved in a mixture of 20ml dichloroethane and 15ml water. A solution of 9.4g (25 mmol) O,O-Dibenzoyl-_2R,3R_-tartaric acid in 40ml of dichloroethane and methanol (see amounts below) was added to the two-phase solution during 30 minutes at room temp. From the stirred solution the crystallization starts in 10-15 minutes. The resulting suspension was stirred at 5°C overnight, then filtered. The precipitate was washed on the filter three times with 5°C dichloroethane and air dried under a heat lamp. The precipitated salt were dissolved in 30ml 2N NaOH and extracted with 3x25ml dichloromethane. After drying over MgSO4, filtering and evaporation of the solvent, the methamphetamine freebase was obtained, which can be dissolved in diethyl ether and bubbled with dry HCl gas to obtain the crystalline hydrochloride salt.
> 
> Using 3ml methanol in the above procedure gave d(+)-methamphetamine in 93% yield and 85% optical purity, and 18.8ml methanol gave 78% yield in 98% optical purity.


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## G.Patton

>O,O-Dibenzoyl-2R,3R-Tartaric Acid
I think it is much hard to find than d-tartaric acid


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## MadHatter

G.Patton said:


> >O,O-Dibenzoyl-2R,3R-Tartaric Acid
> I think it is much hard to find than d-tartaric acid



G.PattonNah. They have it at labarotoriumdiscounter.nl.
Not extremely cheap, but doable. And no end user declaration:








(-)-Dibenzoyl-L-tartaric Acid >98.0%(HPLC)(T) 250g







www.laboratoriumdiscounter.nl


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## Kslzlxczkaoxl

G.Patton said:


> Sorry, I was confused. L(+) isomer can be used to get (-)D-amph/methamph. Procedure a little bit different from mine and you can get another isomer. I worked with D-Isomer only. *You'll get D-amph L-tartaric acid as an precipitate.*



G.PattonSo can we then take this tartrate salt D-Amph L-Tartaric, treat with sodium hydroxide, extract and precipitate with with sulphuric acid?


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## G.Patton

Kslzlxczkaoxl said:


> So can we then take this tartrate salt D-Amph L-Tartaric, treat with sodium hydroxide, extract and precipitate with with sulphuric acid?



Kslzlxczkaoxlyes


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## UWe9o12jkied91d

G.Patton said:


> yes



G.PattonI'm going to buy tartaric acid RIGHT now, thank you based sir


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## workworkwork

G.Patton said:


> Acetic essence is often used to produce hydrogen, but I "start" the reaction to produce hydrogen with water. Less acidic medium, which means less alkali must be added later. ​



G.PattonIn this method is not used acetic acid, but is used another chemical together with p2np in a solution, is that the difference compared to the method used in the 2 videos to make amphetamine from aluminum amalgam?
Im talking about only the first part of the method, production of amphetamine, not about the second, Extraction of d-amphetamine.


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## G.Patton

workworkwork said:


> In this method is not used acetic acid, but is used another chemical together with p2np in a solution, is that the difference compared to the method used in the 2 videos to make amphetamine from aluminum amalgam?



workworkworkHello, almost the same. There is no acetic acid only.


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## finch3523

can somebody explain me again pls what would be the difference if I use l-tartaric instead of d-tartaric acid with freebase? with l-tartaric there would precipate what? the d-amphetamine l-tartaric salt? What would I do then?


----------



## G.Patton

finch3523 said:


> with l-tartaric there would precipate what? the d-amphetamine l-tartaric salt?



finch3523Yes, you are right


----------



## MadHatter

finch3523 said:


> can somebody explain me again pls what would be the difference if I use l-tartaric instead of d-tartaric acid with freebase? with l-tartaric there would precipate what? the d-amphetamine l-tartaric salt? What would I do then?



finch3523GAAAH! Use the right nomenclature with capital letters! Mixing them gets so damn confusing. 

D-(-)- tartaric acid will give you a tartrate salt of D-meth/amph. I honestly don't know what the physical properties of that salt is, how well it stores, melts or tastes. But it should be fully usable.


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## finch3523

which one is the one you can buy everywhere?


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## MadHatter

LOL. 
L-(+)-tartaric acid. 
Sometimes called d-tartaric acid (with a LOWERCASE "d").


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## finch3523

yeah that is the one i am talking about. did you use this one to make dextro-amp?


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## finch3523

with L-(+)-tartaric acid it means you will have dextro amphetamine salt crystallizing or levo? sorry its very confusing.

"You can repeat procedure of cleaning precipitate of l-amphetamine d-tartaric salt by methanol to increase yield."

I want to do that. Can you describe the steps in more detail?


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## MadHatter

finch3523 said:


> with L-(+)-tartaric acid it means you will have dextro amphetamine salt crystallizing or levo? sorry its very confusing.
> 
> "You can repeat procedure of cleaning precipitate of l-amphetamine d-tartaric salt by methanol to increase yield."
> 
> I want to do that. Can you describe the steps in more detail?



finch3523L-tartaric acid will salt out L-amphetamine. Simple as that. 
Mix the tartrate with the racemic freebase and a salt will be created. Thats L-amphetamine tartrate. Filter that out, separate. Repeat a couple of times. Eventually you will have a freebase with mostly D-amphetamine in. Salt THAT out with sulphuric acid (or bubble with dry HCl gas if it's meth) to get your non-racemic product.


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## finch3523

ok. but I want to check it with CAS numbers because I have still conflicting info what yields what salt.

- (the one that comes from fruits and is cheap and available) CAS 87-69-4, L (+) - tartaric acid -> results into ?

(unnatural one and is expensive) CAS 147-71-7, D (-) - tartaric acid -> results into ?


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## Evilcarrot2

Question about p2np to amph.
So I used aluminium granules as I had that laying around.
After I amalgamated it which was deep grey sludge floating around I drained and wash 4 or 5 times added small amount of distilled water and dripped 14%p2np in ipa slowly at 1st but my exotherm wasn't bad 45°c'ish I speeded it up but even after all addition in about 15mins it never went over 55c without cooling, I don't think enough hydrogen was produced from the slow reaction. Could I bubble h2 through mixture from hydrogen generator to make sure I'm using enough hydrogen or have I just fucked it up with granules?
Just wanted to know before I basify


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## G.Patton

Evilcarrot2 said:


> Question about p2np to amph.
> So I used aluminium granules as I had that laying around.
> After I amalgamated it which was deep grey sludge floating around I drained and wash 4 or 5 times added small amount of distilled water and dripped 14%p2np in ipa slowly at 1st but my exotherm wasn't bad 45°c'ish I speeded it up but even after all addition in about 15mins it never went over 55c without cooling, I don't think enough hydrogen was produced from the slow reaction. Could I bubble h2 through mixture from hydrogen generator to make sure I'm using enough hydrogen or have I just fucked it up with granules?
> Just wanted to know before I basify



Evilcarrot2It is better to use Al foil from grocery store for this synthesis way. In case of H2 bubbling, it is better to use Pd/C as catalyst.


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## Evilcarrot2

G.Patton said:


> It is better to use Al foil from grocery store for this synthesis way. In case of H2 bubbling, it is better to use Pd/C as catalyst.



G.PattonI've tried to look but can't really find an answer for pd/c preparation 
I have activated carbon and maybe 50g of palladium chloride made by dissolving palladium in aqua rega and bubbling chlorine through which dropped out a nice dark red salt looks a little like iron oxide. And dried to constant weight. 
How do I make pd/c 
Sorry a bit off topic. 
Is pd/c pyrophoric?


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## UWe9o12jkied91d

Evilcarrot2 said:


> I've tried to look but can't really find an answer for pd/c preparation
> I have activated carbon and maybe 50g of palladium chloride made by dissolving palladium in aqua rega and bubbling chlorine through which dropped out a nice dark red salt looks a little like iron oxide. And dried to constant weight.
> How do I make pd/c
> Sorry a bit off topic.
> Is pd/c pyrophoric?



Evilcarrot2`https://patentimages.storage.googleapis.com/f3/8a/37/258648c5724d09/US3458576.pdf


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## Amphibian

Evilcarrot2 said:


> I've tried to look but can't really find an answer for pd/c preparation
> I have activated carbon and maybe 50g of palladium chloride made by dissolving palladium in aqua rega and bubbling chlorine through which dropped out a nice dark red salt looks a little like iron oxide. And dried to constant weight.
> How do I make pd/c
> Sorry a bit off topic.
> Is pd/c pyrophoric?



Evilcarrot2*Palladium Catalyst Preparation* (haven't tried it out)


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## Evilcarrot2

Wow than



Amphibian said:


> *Palladium Catalyst Preparation* (haven't tried it out)



AmphibianWow thanks exactly what I've been looking for


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## G.Patton

Evilcarrot2 said:


> Is pd/c pyrophoric?



Evilcarrot2I don't think so.


Evilcarrot2 said:


> How do I make pd/c


Wikipedia said:
A solution of palladium chloride and hydrochloric acid is combined with aqueous suspension of activated carbon. The palladium(II) is then reduced by the addition of formaldehyde. Palladium loading is typically between 5% and 10%. Often the catalyst mixture is stored moist. 

I've never prepared Pd/C by myself.


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## diogenes

finch3523 said:


> can somebody explain me again pls what would be the difference if I use l-tartaric instead of d-tartaric acid with freebase? with l-tartaric there would precipate what? the d-amphetamine l-tartaric salt? What would I do then?



finch3523When you switch the tartaric acid isomers, then everything is simply the other way round. The amph isomer which was in the organic phase will be in the water and the salt (water soluble) will be in the organic. I know some people use the L tartaric acid (despite more difficult to get) because then the D amphetamine will be in the water phase.


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## PhantomFeatherSword

Excuse the amateur question, but when I was reading about tartaric acid on Wikipedia, there was a line that confused me a bit:


> Naturally occurring form of the acid is *dextro tartaric acid *or *L-(+)-tartaric acid* (obsolete name _d_-tartaric acid). Because it is available naturally, it is cheaper than its enantiomer and the meso isomer. The _dextro_ and _levo_ prefixes are archaic terms.


When I read the above "dextro tartaric acid *or* L-(+)-tartaric acid", I kinda read it as "dextro tartaric acid* AKA* L-(+)-tartaric acid".
Which makes me wonder, if I'm trying to isolate the _dextroamphetamine_ isomer, should I be buying the _L-(+)-tartaric acid_ (like this)? Or the _D-(-)-Tartaric Acid_ (like this)? Im really hoping it's the D-(-)-Tartaric Acid, because that's what I already have.


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## G.Patton

PhantomFeatherSword said:


> Excuse the amateur question, but when I was reading about tartaric acid on Wikipedia, there was a line that confused me a bit:
> 
> When I read the above "dextro tartaric acid *or* L-(+)-tartaric acid", I kinda read it as "dextro tartaric acid* AKA* L-(+)-tartaric acid".
> Which makes me wonder, if I'm trying to isolate the _dextroamphetamine_ isomer, should I be buying the _L-(+)-tartaric acid_ (like this)? Or the _D-(-)-Tartaric Acid_ (like this)? Im really hoping it's the D-(-)-Tartaric Acid, because that's what I already have.



PhantomFeatherSwordHello, you can use both of them. I wrote the method for L-tartaric acid. Read comments above. Your question is already discussed several times.
Also, read *this* theme.


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## Midget_Impinger

G.Patton said:


> *Extraction of d-amphetamine*​We've got racemic amphetamine. It contains 1 molecule of d-amphetamine per 1 molecule of l-amphetamine. Next, 6 g of racemate is taken and dissolved in 6 ml of water, an alkali solution is added to reach pH = 11.​
> 
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> Spoiler: Pic.17
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> View attachment 1466
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> ​Extract with 5 ml of petroleum ether and warm the solution, add 2.45 g of d-tartaric acid in alcohol solution to the mixture. Then add alcohol until completely dissolved and cool with stirring. The l-amphetamine d-tartaric salt precipitates. The _d-amphetamine_ remains in the solution. You can repeat procedure of cleaning precipitate of l-amphetamine d-tartaric salt by methanol to increase yield.​
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> Spoiler: Pic.18
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> View attachment 3173
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> ​We precipitate d-amphetamine with an additional amount of d-tartaric acid. We filter the precipitate, get the base of d-amphetamine, adding alkali to pH = 11.
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> Spoiler: Pic.19
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> View attachment 1470
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> ​We acidify the d-amphetamine base to pH = 6 with a solution of sulfuric acid in acetone. This gives 2.63 g of d-amphetamine sulfate. Yield is 2.63 / 3 = 87.7%
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> Spoiler: Pic.20
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> View attachment 1471
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> ​This extraction method valid to amphetamine, which was synthesized by any routes. There is another way to obtain dextroamphetamine.



G.Patton@G.Patton - Is this optical resolution process using _d-tartaric acid_ applicable to other amphetamines? Specifically _4-fluoroamphetamine_, _4-fluoromethamphetamine_ and plain ol _methamphetamine_?


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## G.Patton

Midget_Impinger said:


> @G.Patton - Is this optical resolution process using _d-tartaric acid_ applicable to other amphetamines? Specifically _4-fluoroamphetamine_, _4-fluoromethamphetamine_ and plain ol _methamphetamine_?



Midget_ImpingerHello, yes, it is.


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