mithyl2

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when i tried fractional distillation i think some of the water came through with the ipa. and the heat was only at 80c the entire time of the distillation. i've done this a couple of times before where if i leave the distillation going i'll just end up with the copper as a solid goo, and no liquid.
i'll precipitate the amphetamine asap and see what the product is like, as maybe the ipa was present as a contaminant in previous batches.

are there any suggestions on what i can do to make sure i get only the ipa, and none of the water containing amphetamine?

i'll be trying variations of this synthesis as well.
 

OrgUnikum

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when i tried fractional distillation i think some of the water came through with the ipa. and the heat was only at 80c the entire time of the distillation. i've done this a couple of times before where if i leave the distillation going i'll just end up with the copper as a solid goo, and no liquid.
i'll precipitate the amphetamine asap and see what the product is like, as maybe the ipa was present as a contaminant in previous batches.

are there any suggestions on what i can do to make sure i get only the ipa, and none of the water containing amphetamine?

i'll be trying variations of this synthesis as well.
mithyl2IPA forms an azeotrope with water so all IPA you distill will have about 30% water in it. You can distill the IPA off without the possibility to have some amphetamine coming over either by vacuum distillation, only a little vacuum like an aspirator pump produces is sufficient, say, when you have have the IPA coming at 60 °C or less there will be no amphetamine in it. Or you render the reaction acidic by adding diluted acetic acid until ph is 3 or less. The amphetamine will form a salt and not distill. Let cool down, then add ice-cold 10% NaOH solution until ph 12 and steamdistill the Amphetamine base.

It must be told, that the addition of 20% NaOH "to basify the reaction" is completely bs as if you measure it you will find the reaction is already alkaline like hell, ph 12 or more as the NaBH4 and its products are all strong bases. Why it is in the original text I cannot fathom, why it was posted here, well.... This happens if you lift something from an article or here thesis 1 to 1 without really knowing or trying. See attached document page 20 and page 30, on page 30 you will find the procedure word by word.
The problem is obvious: You have a mixture of water and IPA and Amphetamine. You could add brine and so salt the IPA with the Amph out, that would work well. But adding NaOH 20% will not suffice to salt the IPA out but in the best case some Amph will come to the top and this will contain IPA. Or you extract IPA and Amph with a water insoluble nonpolar solvent. This works also well. Or do as described above. In any case, check the ph and you will find that NaOH to make it more basic/alkaline is just not necessary.
Generally IPA as solvent for extracting something from water works only if the water layer is completely saturated by salts like NaCl for example, by something what is NOT also soluble in IPA like NaOH.

See page 20 and page 30 of the attached thesis by Jademyr
 

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mithyl2

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IPA forms an azeotrope with water so all IPA you distill will have about 30% water in it. You can distill the IPA off without the possibility to have some amphetamine coming over either by vacuum distillation, only a little vacuum like an aspirator pump produces is sufficient, say, when you have have the IPA coming at 60 °C or less there will be no amphetamine in it. Or you render the reaction acidic by adding diluted acetic acid until ph is 3 or less. The amphetamine will form a salt and not distill. Let cool down, then add ice-cold 10% NaOH solution until ph 12 and steamdistill the Amphetamine base.

It must be told, that the addition of 20% NaOH "to basify the reaction" is completely bs as if you measure it you will find the reaction is already alkaline like hell, ph 12 or more as the NaBH4 and its products are all strong bases. Why it is in the original text I cannot fathom, why it was posted here, well.... This happens if you lift something from an article or here thesis 1 to 1 without really knowing or trying. See attached document page 20 and page 30, on page 30 you will find the procedure word by word.
The problem is obvious: You have a mixture of water and IPA and Amphetamine. You could add brine and so salt the IPA with the Amph out, that would work well. But adding NaOH 20% will not suffice to salt the IPA out but in the best case some Amph will come to the top and this will contain IPA. Or you extract IPA and Amph with a water insoluble nonpolar solvent. This works also well. Or do as described above. In any case, check the ph and you will find that NaOH to make it more basic/alkaline is just not necessary.
Generally IPA as solvent for extracting something from water works only if the water layer is completely saturated by salts like NaCl for example, by something what is NOT also soluble in IPA like NaOH.

See page 20 and page 30 of the attached thesis by Jademyr
OrgUnikumAfter I added the CuSO4*5H2O and then held the solution at 80c for 30 minutes, I added hydrochloric acid in the absence of acetic acid (that should be ok?) so the solution reached ph 2, and then I used simple distillation to distill off the IPA between the temps of 83C - 91C (although virtually nothign came over past about 87c), then cooled down the solution, filtered it, then added the aqueous NaOH. Now at this point I'll steam distill the amphetamine out. Do let me know if there's anything wrong with the order of things here. (I don't think I needed to filter the solution and I'll need to reflux the solution for about 3 hours instead of holding it at 80C for 30 mins.)

When I filtered the solution to separate the copper complex and I added the aqueous NaOH and the solution turned dark murky brown and smelled a little of fish with a ph of 11, and the copper was a green cake substance. I'll add more aqueous NaOH to increase to ph 12, then I'll steam distill from here. (No layers formed upon the naoh addition, so it appears i've got rid of all of the ipa from the solution.)

might toluene be a good candidate for a water insoluble nonpolar solvent?

With regards to basifying the reaction, are you saying that 20% NaOH is overkill, and that 10% will do?
 

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After I added the CuSO4*5H2O and then held the solution at 80c for 30 minutes, I added hydrochloric acid in the absence of acetic acid (that should be ok?) so the solution reached ph 2, and then I used simple distillation to distill off the IPA between the temps of 83C - 91C (although virtually nothign came over past about 87c), then cooled down the solution, filtered it, then added the aqueous NaOH. Now at this point I'll steam distill the amphetamine out. Do let me know if there's anything wrong with the order of things here. (I don't think I needed to filter the solution and I'll need to reflux the solution for about 3 hours instead of holding it at 80C for 30 mins.)

When I filtered the solution to separate the copper complex and I added the aqueous NaOH and the solution turned dark murky brown and smelled a little of fish with a ph of 11, and the copper was a green cake substance. I'll add more aqueous NaOH to increase to ph 12, then I'll steam distill from here. (No layers formed upon the naoh addition, so it appears i've got rid of all of the ipa from the solution.)

might toluene be a good candidate for a water insoluble nonpolar solvent?

With regards to basifying the reaction, are you saying that 20% NaOH is overkill, and that 10% will do?
mithyl2Any concentration of NaOH will do as long you get to ph 12. More diluted like 10% and cold from the fridge is better and adding it to the reaction which has cooled down too as it easily possible to burn, say destroy some of your product by adding strong lye to a hot A-solution. Same for adding acid, diluted and cold. If your HCl was diluted and everything coldish at least then it will be fine.
Well yes, fish it is, thats the smell of A.
You want the solution you steamdistill at ph 12 but not choke-full with NaOH as otherwise when the water gets less one easily blows over some NaOH and this you do not want in your A. The filtration is done as it sems some Boron stuff likes to steamdistill over - this you also do not want.
 

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Any concentration of NaOH will do as long you get to ph 12. More diluted like 10% and cold from the fridge is better and adding it to the reaction which has cooled down too as it easily possible to burn, say destroy some of your product by adding strong lye to a hot A-solution. Same for adding acid, diluted and cold. If your HCl was diluted and everything coldish at least then it will be fine.
Well yes, fish it is, thats the smell of A.
You want the solution you steamdistill at ph 12 but not choke-full with NaOH as otherwise when the water gets less one easily blows over some NaOH and this you do not want in your A. The filtration is done as it sems some Boron stuff likes to steamdistill over - this you also do not want.
OrgUnikumok. I'm steam distilling (or trying to) as I'm type this. A problem i'm having is the enormous fluctuation in the temperature of the steam. a change in 1 degree on the mantle can increase or reduce by 15+ degrees on the steam.

I think the fishy smell is the naoh, (it is the same as when i attempted a dmt extraction).
 

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ok. I'm steam distilling (or trying to) as I'm type this. A problem i'm having is the enormous fluctuation in the temperature of the steam. a change in 1 degree on the mantle can increase or reduce by 15+ degrees on the steam.

I think the fishy smell is the naoh, (it is the same as when i attempted a dmt extraction).
mithyl2The steam-temperature should be 94 to 98 °C you can hardly get over 100 °C so if it boils it will make steam and the steam has 94 °C+ with A and 99-100 °C with plain water.

NaOH has no smell, NaOH vapors are extremely caustic you will feel it when it eats your face.
Amines are the ones with the rotting fish stink.
 

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Hello,
Can sodium borohydride in this experiment be replaced with cas25895-60-7 Sodium cyanoborohydride?
 

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Hello,
Can sodium borohydride in this experiment be replaced with cas25895-60-7 Sodium cyanoborohydride?
ethanaaaCyanoborohydride is very well suited for reductive aminations as it does not reduce ketones, say its less powerful then NaBH4. It is also prone to release cyanide on contact with acids and it is quite expensive. It might be just able to do the job here if in combination with Nickel Chloride, with Cu(II) I have my doubts and think rather not. It makes little to no sense to try to use it for this reaction.
 

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Which PH it should have ?
Do the PH say something about the quality ?
 

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Can I replace CuCl2 with CuSO4. I read it on reddit and idk if is this possible but I think yes bc Cu(II) I am right?
 

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Can I replace CuCl2 with CuSO4. I read it on reddit and idk if is this possible but I think yes bc Cu(II) I am right?
T0lek511Yes you should be able to. Although I'm having troubles with this synthesis myself, so perhaps I should try CuCl2 instead. It's much more expensive and much less widely available though
 

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Yes you should be able to. Although I'm having troubles with this synthesis myself, so perhaps I should try CuCl2 instead. It's much more expensive and much less widely available though
mithyl2CuSO4 works the same or better then CuCl2, you need to use a little bit more though as the pentahydrate of trade is heavier (per copper atom) then the CuCl2 dihydrate. To be precise, you have to multiply the number for the CuCl2.2H2O by 1,5 to get the right amount of CuSO4.5H2O.

Your problems are caused by something else.
Here somebody claiming >90% yield:
....so gave the reaction another try with iPrOH. I got a clear biphasic reaction again but apparently that is how it is supposed to be as I got a 91% yield. I used two times 16 gram NaBH4 contrasting a bit of NaOH on 20 gram PN2P and heated the mixture to 50 degrees before adding 2 grams of CuCl2 dissolved in 10/4 iPrOH/water, I guess about 20ml of that.

The reaction was refluxed for one hour (and worked up)
iPRrOH is IPA
Please note that he adds NaOH - this should be done always if one uses water, methanol or ethanol in the reaction, as all of those react with borohydride, this reaction is partially suppressed by a strong base. Thats the reason why NaBH4 reactions in methanol are usually done at 0° to 5°C.
I also think he adds water only with the second borohydride before the copper salt. In this case the NaOH should be added then. If the copper salt turns light blue - thats ok too, this is copper hydroxide and carbonate, both work all the same.

It is not my procedure, but I am sure it works, 91% yield though? Rather not.
....
 

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@G.Patton
Hi. Can I use 15% sulphuric acid for making amp sulphate from freebase? In Czech Republic sulphuric acid is very restricted.
 

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@G.Patton
Hi. Can I use 15% sulphuric acid for making amp sulphate from freebase? In Czech Republic sulphuric acid is very restricted.
T0lek511Hello, you can try. Take into account that your amphetamine sulphate will be dissolved in water of this solution.
 
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Hello, you can try. Take into account that your amphetamine sulphate will be dissolved in water of this solution.
G.PattonThank you for your quick reply. One more question @G.Patton Can I use CuSO4 * 5H2O instead CuCl2 anhydrous? (as is in original synthesis). I think yes but I am very interested in your opinion. If answer is yes, how can I do calculation?
 

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Thank you for your quick reply. One more question @G.Patton Can I use CuSO4 * 5H2O instead CuCl2 anhydrous? (as is in original synthesis). I think yes but I am very interested in your opinion. If answer is yes, how can I do calculation?
T0lek511I don't think so, you cannot.
 

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Hi. Can I use normal evaporation of ipa in step 8 without vacuum? I mean I heat it and IPA will be boiled without vacuum.
T0lek511Hello, yes, you can. Do not overheat the solution. In opposite case you'll loose the yield.
 

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Hello, you can try. Take into account that your amphetamine sulphate will be dissolved in water of this solution.
G.PattonIf there's already water in the solution that the amphetamine is being precipitated from (as in the video), would this additional water present in the acid matter?
 

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Thank you for your quick reply. One more question @G.Patton Can I use CuSO4 * 5H2O instead CuCl2 anhydrous? (as is in original synthesis). I think yes but I am very interested in your opinion. If answer is yes, how can I do calculation?
T0lek511Yes. Any Cu(II) salt can be used. The amount of CuSO4.6H2O needed would be about twice as much as anhydrous CuCl2.
 

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If there's already water in the solution that the amphetamine is being precipitated from (as in the video), would this additional water present in the acid matter?
mithyl2Hi, it's worth to get rid of water cuz amphetamine sulphate (resulting salt) is soluble in water and it's much easier for you to carry out precipitation without water. In case you cannot do this, you should evaporate water after precipitation to get dissolved in water amphetamine sulphate.

Edit: sorry, I thought we are talking about meth. %)
 
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Hi, it's worth to get rid of water cuz methamphetamine hydrochloride (resulting salt) is soluble in water and it's much easier for you to carry out crystallization without water. In case you cannot do this, you should evaporate water after crystallization to get dissolved in water methamphetamine hydrochloride.
G.PattonSo an extraction would be in order prior to precipitation to both get rid of the water and keep the amphetamine?

What do you recommend I do to get pure sulfuric or phosphoric acid? because I can't seem to find any sellers of acids, and domestic purchases aren't possible at the moment.
 

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Hello, H2.

It isn't possible, don't worry.
G.PattonSo for safety is better use electric heater than propane-butane? How much hydrogen is made? Littlebit or much? The problem is I have only propane-butane heater, I will do only about 20g of P2NP. Is in this scale dangerous to use propane-butane heater?
 

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So for safety is better use electric heater than propane-butane? How much hydrogen is made? Littlebit or much? The problem is I have only propane-butane heater, I will do only about 20g of P2NP. Is in this scale dangerous to use propane-butane heater?
T0lek511
>So for safety is better use electric heater than propane-butane?
Yes, of course
How much hydrogen is made? Littlebit or much?
You can calculate this according to the reaction equation and the molar constant of the gas (22.4 l/mol).
Is in this scale dangerous to use propane-butane heater?
I strongly do not recommend to use open flame because you'll get hydrogen and your lab can explode.
 

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@G.Patton
Hi. Can I use 15% sulphuric acid for making amp sulphate from freebase? In Czech Republic sulphuric acid is very restricted.
T0lek511You have to concentrate it. By heat it up for hours :) I know the problems :D
Check it by density!
 
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