Same goes for meth, but I think separating by precipitation is not as effective with meth as using the different solubilities in methanol of the two tartaric diastereomers.
So you acidify the racemic freebase with racemic tartrate (both D and L), precipitating D and L-meth tartrate.
Then you recrystallize those salts from methanol. L-meth tartrate is much more soluble in methanol and will stay in solution while D-meth crashes out and can be collected.
I have been following a professional chemist doing clandestine work on a smaller forum, and he has been working intensively with resolution of amphetamines for a while. let's just say itisn't really as easy as it seems. It won't be 100 %, you're lucky to reach 80, you'll loose product, and the only way to know for sure how well you did is by buying a polarimeter- either an automatic one for €10-20.000 or a cheaper manual one that takes forever to learn how to calibrate and master.
Why did some 'specialized' chemists, specialized as they don't use the common method of platinum and hydrogen but respectively with Al/Hg and other one with nickel and hydrogenation, ask me specially for d-(-)-tartaric acid?
Is that because they more likely get a higher optical purity or ?
I am trying to find out why
Think so I'm not ,,100%percent sure but I think you get more return and less problems getting the dmeth out especially when the using sodium borohydride
Available in my country L (+) tartaric acid Is the procedure the same or has the state of sedimentation changed some addition Where does dextromethamphetamine go in the solution or does it precipitate
Available in my country L (+) tartaric acid Is the procedure the same or has the state of sedimentation changed some addition Where does dextromethamphetamine go in the solution or does it precipitate
Why don't you look in forum threads and you might find it if you took the time to look instead of being spoon feed all the time
Isomers and tartaric acid you lazy bastard.
Indeed, I have researched and understood that there are two ways to go for the isomer, one is in the solution and the second is precipitated, and vice versa. I am lazy. I do not have a girl to sleep with.
For MDMA scheme is moles of freebase 1:1 moles of tartaric solution, if you use L-tartaric the must keep the solid precipitate, the liquid part has the enantiomer and salt not desired.
You must solve and set alkali 12-13 ph the solid precipitate to make fb appears.
This fb is with the enantiomer that you want isolated.
The liquid part could be alkalinized but adding enough water too to get the fb of the other enantiomer if you want to mix them in ratios.
I can test it next week but is in this way.
I tried to rethink all I read here about isomers separation, and it looks you are totally right: the best way is to do it in water.
Just one thing is bothering: if we use FB and tartaric in molar proportions 1:1 there will be an excess of unreacted tartaric in bottom layer together with precipitated tartrate.
Wont this unreact tartaric give me more impurities when FB extracted from precipitates by alkali?
I never used digital PH meter. Does it worth to control PH of bottom layer using such device while tartaric added to reach PH 4-5 in this layer?
Did try S newly separated from your racemic. Difficult to say, how pure is this S, but effect is distinguishable different.
First of all, it has much less stimulating effect: all is about emotions.
Also detected: much less bruxism (me personally didn't feel any bruxism at all), less sweating, less confusion.
I can say, for the regular racemic consumer it may look less powerful as it has almost zero stimulant. From the other side, it is a pure antidepressant that you may take in the morning and go to the office to do your usual work without the risk of being discovered as a stoned junky.
Did try S newly separated from your racemic. Difficult to say, how pure is this S, but effect is distinguishable different.
First of all, it has much less stimulating effect: all is about emotions.
Also detected: much less bruxism (me personally didn't feel any bruxism at all), less sweating, less confusion.
I can say, for the regular racemic consumer it may look less powerful as it has almost zero stimulant. From the other side, it is a pure antidepressant that you may take in the morning and go to the office to do your usual work without the risk of being discovered as a stoned junky.
For MDMA scheme is moles of freebase 1:1 moles of tartaric solution, if you use L-tartaric the must keep the solid precipitate, the liquid part has the enantiomer and salt not desired.
You must solve and set alkali 12-13 ph the solid precipitate to make fb appears.
This fb is with the enantiomer that you want isolated.
The liquid part could be alkalinized but adding enough water too to get the fb of the other enantiomer if you want to mix them in ratios.
I can test it next week but is in this way.
Is about solubility but I'm sure that methanol is only useful when you are using D-tartaric or DL tartaric, using L-tartaric is more easy with water I did it many times.
700gr+1.4L water
972gr FB
Works fine, the new improvement is that now I know is important to do it several times until no oil appears when turns liquid layer alkali.
Methanol and tartaric are mixed until complete dissolution, freebase is added while stirring and continue stirring vigorously 2-3min.
Let it at RT during 24 hours until the complete solid mass is formed(if in a couple of hours no solids are formed you should stir it again)
It's filtered and now are exactly the same steps as the other method.
- In the liquid part once I had all the DCM extractions I decided to make an acid-base washing, even the DCM color looks cleaner than the other one, to avoid to be "dirty" like the first method happened and I obtained 10gr of D-meth absolutely clean and pure(pic link at the bottom)
- In the solid part 13gr of enough clean L-meth freebase without acid-base washing obtained.
- Cleaning issue could be fixed during the crystallization stage too are many ways.
Obviously is very difficult to check how much D or L are in reality in the stuff only with Chiral analysis not easy accessible.
I also know that it is not the most correct to compare two methods using some different reagents but in reality they do practically the same function in the process.
In short, similar methods and yields the main differences are that in the second one you can avoid the reflux(so could be easier) and the final freebases looks cleaner than the others method.
When I will have free time again like this weekend(unfortunately not usual :-( only will be remaining to test in small scale the"mexican"method for meth isomer separation is quite different and I only did it in big scale although I finally decided to use the method explained for big scale too.
These would be the 3 methods that I did and I can talk about them with experience.
About when and how to make an acid-base washing instead steam distillation...etc etc needs a complete and long post the same for crystallization.
I'm thinking to post all the possible and more profitable options during the route from BMK(5449) to D-Meth HCL but this would be a long work and I don't know when I will have enough time again hahah at least is planned.
I got total fault here, but any way, posting the report for further analysis.
I had 37 gr of MDMA FB after ABE washing at the beginning.
L tartaric CAS 87-69-4 34 in 26 gr were dissolved in Methanol 340 ml, it refers to molar proportions 1(FB) : 0.9(tartaric).
After FB added, it was stirred in the flat bottom flask for a while 1500 RPM and left for overnight.
In the morning flask checked, but nothing happened. I added 8 gr of L tartaric extra to adjust proportions to 1:1.2 as suggested by @btcboss2022 but got fault again.
So I decided to evaporate some methanol in crystallizer under the hood.
Hotplate surface was heated up to 70C and 2L crystallizer on such temperature evaporates methanol 2.0-2.5 gr per 1 min.
It was evaporated till 150 ml left (calculated by weight) and set in the round bottom flask for another attempt of crystallization. But nothing happened again.
I don't know what I did wrong or my hands growing from my ass. But I decided to evaporate all the methanol (it is not difficult as this shit is extremely volatile) and separate freebase leftovers from salt with p.ether.
I got total fault here, but any way, posting the report for further analysis.
I had 37 gr of MDMA FB after ABE washing at the beginning.
L tartaric CAS 87-69-4 34 in 26 gr were dissolved in Methanol 340 ml, it refers to molar proportions 1(FB) : 0.9(tartaric).
After FB added, it was stirred in the flat bottom flask for a while 1500 RPM and left for overnight.
In the morning flask checked, but nothing happened. I added 8 gr of L tartaric extra to adjust proportions to 1:1.2 as suggested by @btcboss2022 but got fault again.
So I decided to evaporate some methanol in crystallizer under the hood.
Hotplate surface was heated up to 70C and 2L crystallizer on such temperature evaporates methanol 2.0-2.5 gr per 1 min.
It was evaporated till 150 ml left (calculated by weight) and set in the round bottom flask for another attempt of crystallization. But nothing happened again.
I don't know what I did wrong or my hands growing from my ass. But I decided to evaporate all the methanol (it is not difficult as this shit is extremely volatile) and separate freebase leftovers from salt with p.ether.
Seems something wrong with your tartatic no other explanation.
For 37gr of MDMA freebase try with 35gr of tartaric solved in 70ml of methanol or water.
Seems something wrong with your tartatic no other explanation.
For 37gr of MDMA freebase try with 35gr of tartaric solved in 70ml of methanol or water.
No, I do it every week in that way in the last year with water with dextrotartaric and with methanol with levotartaric in the same ratios and works perfectly I will make pics.
Interesting. I did this tartaric separation three times.
First two times in was done in water, and the solution turns red without boiling immediately.
But third time, when I got fault, it was done in methanol. The difference - it didn't turn red. But the acid was from different batch. And yes, I did try to keep the flask in the freezer as well. Zero result.
So, I don't know what is wrong. May be tartaric was improper or something else?
Seems something wrong with your tartatic no other explanation.
For 37gr of MDMA freebase try with 35gr of tartaric solved in 70ml of methanol or water.
No, I do it every week in that way in the last year with water with dextrotartaric and with methanol with levotartaric in the same ratios and works perfectly I will make pics.
Sounds like a stupid question, but could it be that meth tartrate is less soluble in methanol than mdma?
I tried to read on the topic of solubility, and found only very conflicting information. It seems that people are just fantasizing about tartrate solubility.
I will try with ethanol as soon I get inspiration or do base extraction.
Interesting. I did this tartaric separation three times.
First two times in was done in water, and the solution turns red without boiling immediately.
But third time, when I got fault, it was done in methanol. The difference - it didn't turn red. But the acid was from different batch. And yes, I did try to keep the flask in the freezer as well. Zero result.
So, I don't know what is wrong. May be tartaric was improper or something else
I didn't check ph of base itself, but it was after ABE and probably shall be around 12.
When I did separation in water, I simply added tartaric water liquid in small portions, and watching as FB layer decreases small by smaller and checked ph of lower layer with pasteur till it reaches 3-4. As I remember, in molar proportions it was around 1(FB):0.7-0.8(acid)
But I didn't check ph when worked with tartaric methanol as no sense: there is excess of acid. Obviously it shall be below 6.
How do you make methamphetamine HCL from pseudoephendrine into clear crystals and not powder?
Does it have to be re-crystallized with ethanol like in the video?
How do you make methamphetamine HCL from pseudoephendrine into clear crystals and not powder?
Does it have to be re-crystallized with ethanol like in the video?
How do you make methamphetamine HCL from pseudoephendrine into clear crystals and not powder?
Does it have to be re-crystallized with ethanol like in the video?
yes , you can recrystallize in the same way like in the video
Don't get this bullshit motion.ig you had your product you will get shards yes it is possible but you have to use Freon as your solvent when you had it it will form shards buy if you use the yeh normal solvents eg toluene you will get powder which has to recrystallised
When you guys are thinking about this racemization and talking about ph, what you should be talking about is pka. If you want anything useful from measuring the ph, you have to know the pka. When your ph matches you pka, 50% is acid and 50% is base. 2 points above your pka is the complete neutralized base and 2 points below and you have 100% Lewis acid. That's what I read, if someone disagrees with that, correct me. I will dig up the reference
It's not my method, the method says 85 parts of freebase, 100 parts of tartaric and 1000 parts of methanol. If I'm not wrong is based in 1:1 moles of freebase and tartaric.
is it allowed though to measure methanol in ml and other components in grams? or in this case some 20% variation isnt enough to impact as this is already in excess methanol?
Seems something wrong with your tartatic no other explanation.
For 37gr of MDMA freebase try with 35gr of tartaric solved in 70ml of methanol or water.
Seems something wrong with your tartatic no other explanation.
For 37gr of MDMA freebase try with 35gr of tartaric solved in 70ml of methanol or water.
I've recently finished isomers resolution in acetone, and it looks mdma s-tartrate is bonded with unreact r-base, that doesn't allow solids precipitate.
I've recently finished isomers resolution in acetone, and it looks mdma s-tartrate is bonded with unreact r-base, that doesn't allow solids precipitate.
Could you folks tell me what is the meaning of reflux here? Reaction of tartaric with base is pretty exothermic itself. So, why reflux is done here? Sorry for stupid question.
what exactly does that mean "aqueous methamphetamine hydrochloride solutions" ?
someone please correct me if I'm wrong, I'm not sure if I understand this correctly.
this video is actually preceded by a process, for example, from P2P via Al/Hg.
that is, in the last steps, when we extract, for example, with dichloromethane, I gasify it with hclgas and evaporate dcm. then this resulting meth hydrochloride in this case on the video is 131.8g of meth hcl, I dissolve it in H2O, so I add H2Oto 300g and that's the one "aqueous methamphetamine hydrochloride solutions" and I can now proceed with the synthesis with tartaric acid to D-meth.
what exactly does that mean "aqueous methamphetamine hydrochloride solutions" ?
someone please correct me if I'm wrong, I'm not sure if I understand this correctly.
this video is actually preceded by a process, for example, from P2P via Al/Hg.
Hello, aqueous methamphetamine hydrochloride solution mean methamphetamine hydrochloride, dissolved in water (solvent). Yes, there is written that it was taken from mother liquors (0:23) from meth synthesis (of course, I assumed that it's obvious).
that is, in the last steps, when we extract, for example, with dichloromethane, I gasify it with hclgas and evaporate dcm. then this resulting meth hydrochloride in this case on the video is 131.8g of meth hcl, I dissolve it in H2O, so I add H2Oto 300g and that's the one "aqueous methamphetamine hydrochloride solutions" and I can now proceed with the synthesis with tartaric acid to D-meth.
You can skip acidification step (last step of meth*HCl formation) and continue from distillation of meth free base directly like in video. In this case, you don't need to add alkali.
Could you folks tell me what is the meaning of reflux here? Reaction of tartaric with base is pretty exothermic itself. So, why reflux is done here? Sorry for stupid question.
I don't remember what exactly I was thinking about by that time.
Probably the question is why they heating metanol and d-tartrate up with reflux? Does d-tartrate solubility in metanol go down if T grow up?
I don't remember what exactly I was thinking about by that time.
Probably the question is why they heating metanol and d-tartrate up with reflux? Does d-tartrate solubility in metanol go down if T grow up?
Sorry for the long reply, I haven't seen your question. Sure, solubility always increases at increased temperature. P.S. there is ethanol. The reflux is needed for a complete dissolution and salt formation.
Sorry for the long reply, I haven't seen your question. Sure, solubility always increases at increased temperature. P.S. there is ethanol. The reflux is needed for a complete dissolution and salt formation.
Not always. I noticed solubility of L-tartaric in acetone slightly goes down if T grows more than 15C. I guess, my question was about something like this.
When I did MDMA tartrate separation I did it in acetone, and I noticed tartrate salt builds a kind of colloid with unreacted base. So I had to add more acetone to get salt precipitated. Is there something similar in this process for meth?
Not always. I noticed solubility of L-tartaric in acetone slightly goes down if T grows more than 15C. I guess, my question was about something like this.
When I did MDMA tartrate separation I did it in acetone, and I noticed tartrate salt builds a kind of colloid with unreacted base. So I had to add more acetone to get salt precipitated. Is there something similar in this process for meth?
When I did MDMA tartrate separation I did it in acetone, and I noticed tartrate salt builds a kind of colloid with unreacted base. So I had to add more acetone to get salt precipitated. Is there something similar in this process for meth?
Actually S+ mdma hcl builds colloid with water as well. Probably it is a special property of any salt of mdma isomer due to complicated molecula sceleton.
in general, I did the separation of isomers using dl and L-tartaric acid, gave it to people to try and they said that it was not as strong a meth as with ephedrine, so I believe that it does not separate the racemate
in general, I did the separation of isomers using dl and L-tartaric acid, gave it to people to try and they said that it was not as strong a meth as with ephedrine, so I believe that it does not separate the racemate
No. With tartaric recrystallization with l+ some d crystalizes with it it and with d- some l+ crystallise with it.
With l+ you don't get yields basically above 450 grams.
Also most people use only water, seeing tested papers on internet to have a 100 or as close to 100 optical yield (thus proper seperating) you need some solvent based of a mixture. If I recall it it was water and alcohol but don't know the ratios I must search it and take the chart was a amine tested with multiple solvents
I want a high yield method, and the product can be stored for a long time, say 6 or 12 months. Because there is a method to make the product will be wet, crystallized product is not strong enough, it is easy to break.
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.
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.
Please what is temperature for reaction of tartaric acid, freebase and methanol to separate the isomer, or we should just increase heat until solid dissolves
Ah at 10:37 you filtered d-meth solution and there is residue left somewhere? that you didn't show can be this residue used again? (saturating with hlc gas or?)
Jangan tertipu oleh gerakan omong kosong ini. Jika Anda memiliki produk, Anda akan mendapatkan pecahan. Ya, itu mungkin, tetapi Anda harus menggunakan Freon sebagai pelarut. Ketika Anda memilikinya, itu akan membentuk pecahan. Namun, jika Anda menggunakan pelarut normal, misalnya toluena, Anda akan mendapatkan bubuk yang harus direkristalisasi.
