Example of isomer separation for Meth

[btcboss2022]

Hello,

After receive and see many questions about Meth resolution process I decided to show you an example with my own pics(not professional ones as you will see hahaha):

- 3.65L of "dirty" freebase(just separated and dried after hydrolysis process)
View attachment 20692

- 5.11L of water
View attachment 20693

- 2.55kg of L-tartaric acid(dextro-tartaric acid, d-tartaric acid)
View attachment 20694

- Mix the L-tartaric with the water until all dissolved
View attachment 20695

- Add the freebase to the mixture while vigorous stirring
View attachment 20696
View attachment 20697

- After around 2 min stirring the mixture is hot and becomes thick and later a solid mass
View attachment 20698

Now the process is practically finished just leave it at RT 24 hours and filter it with vacuum.
D-meth freebase will appears after after turning the liquid part alkaline(PH 13).

I hope this help you ;-)

btcboss2022It works with MDMA freebase and Ketamine freebase too just changing ratios with molar weight of each freebase. Remember that in the MDMA and Ketamine case the interesting isomer will be in the solid part using these reagents ;-)

 

[riahisunak]

It works with MDMA freebase and Ketamine freebase too just changing ratios with molar weight of each freebase. Remember that in the MDMA and Ketamine case the interesting isomer will be in the solid part using these reagents ;-)

btcboss2022Hi,
You said this would work with MDMA and ketamkme , just use molar equivalents .
But your ratios don't match the the molar equivalents
3650÷149.2337=24.5 moles
24.5×150.09= 3670g of L tartaric
150.09mm L tartaric
149.2337mm M
??

 

[Sjeik]

It has to be like this..

 

[hunter12]

It has to be like this..

View attachment 40157 View attachment 40157

SjeikNice, you used the same method?

 

[Sjeik]

The initial free base pH is 11?
What is the pH value after mixing?

How many D methyl groups do you get after separation?

qwe111I had like 700ml racemic fb, And after sepration got around 320ml d-fb.

 

[qwe111]

I had like 700ml racemic fb, And after sepration got around 320ml d-fb.

SjeikHey man, this yields great!
Did you clean the L-fb and L-tartaric acid mixture inside the funnel during vacuum filtration? If so, what cleaning do you use? Then how to detach D-fb

 

[Sjeik]

Hey man, this yields great!
Did you clean the L-fb and L-tartaric acid mixture inside the funnel during vacuum filtration? If so, what cleaning do you use? Then how to detach D-fb

qwe111No, i use an centrifuge

 

[Fringg]

No, i use an centrifuge

SjeikPlease, what kind of centrifuge do you use? I tried filtering using reduced pressure and a Buchner funnel, but the tartrate was still wet at the end and retained liquid. I got a little D-isomer at the end

 

[Fringg]

Hello, I greet you all. I want to share with you my experience with the separation of isomers using L-wine. I did three tests. 2x using methanol when I changed the ratio of free base methanol and tartaric acid in both tests. Both tests turned out basically the same, after combining the ingredients and mixing, a solid mass precipitated, which I filtered after 24 hours. As for the appearance of the product and the overall split isomers, perhaps there was a little more products in one test than in the other test. From 30ml of free base I got about 9 grams of d-meth. During evaporation, when the crystals started to appear, it looked good at first, small needles were formed here and there, but the drier it got, the more it resembled a racemate (ugly amorphous substance). When it dried completely, in terms of appearance, I could not tell the difference between the racemate and this divided product. When it was put on foil and warmed up a little, it was obvious that the crystals crystallize a little faster after dissolution than when it is done with the racemate. From this I concluded that some division took place, but not enough. I note that I did not wash the tartrate powder during filtering. It was not written in the procedure, so I preferred not to do it. Well, now we come to the third test, which I did with the help of water according to the btcboss procedure. After combining all the ingredients and mixing vigorously, after a while I got a thick, really thick mass resembling some kind of cream. It had a consistency basically like the photo that was added by the user Sjeik a couple of posts above mine. I closed the container and let it sit for 24 hours, then I put this substance in the filter and spread it over the vacuum filter and turned on the suction. This thick cream-like substance was really difficult to filter, also in the procedure there was nothing written about washing the tartrate in the filter, so I didn't do it. I only got 11 grams of product from 60ml of free base. But the crystals that arrived were transparent and beautiful. I tried melting them on tin foil to see how fast they solidify and it was really fast like pseudoephedrine meth. So I think that the Split izomer was successful except for the mass tragedy of only 11 grams. The problem was probably mainly that I had a bit of a problem during filtration with the fact that the funnel on the suction flask did not seal well and it might also help to wash off the tartrate salt during filtration, but please advise me how much water I can use for this so as not to disturb the solubility of the tartrate in water and thus did not get L isomers into the product. Well thank you

 

[Acab1312]

Hello, I greet you all. I want to share with you my experience with the separation of isomers using L-wine. I did three tests. 2x using methanol when I changed the ratio of free base methanol and tartaric acid in both tests. Both tests turned out basically the same, after combining the ingredients and mixing, a solid mass precipitated, which I filtered after 24 hours. As for the appearance of the product and the overall split isomers, perhaps there was a little more products in one test than in the other test. From 30ml of free base I got about 9 grams of d-meth. During evaporation, when the crystals started to appear, it looked good at first, small needles were formed here and there, but the drier it got, the more it resembled a racemate (ugly amorphous substance). When it dried completely, in terms of appearance, I could not tell the difference between the racemate and this divided product. When it was put on foil and warmed up a little, it was obvious that the crystals crystallize a little faster after dissolution than when it is done with the racemate. From this I concluded that some division took place, but not enough. I note that I did not wash the tartrate powder during filtering. It was not written in the procedure, so I preferred not to do it. Well, now we come to the third test, which I did with the help of water according to the btcboss procedure. After combining all the ingredients and mixing vigorously, after a while I got a thick, really thick mass resembling some kind of cream. It had a consistency basically like the photo that was added by the user Sjeik a couple of posts above mine. I closed the container and let it sit for 24 hours, then I put this substance in the filter and spread it over the vacuum filter and turned on the suction. This thick cream-like substance was really difficult to filter, also in the procedure there was nothing written about washing the tartrate in the filter, so I didn't do it. I only got 11 grams of product from 60ml of free base. But the crystals that arrived were transparent and beautiful. I tried melting them on tin foil to see how fast they solidify and it was really fast like pseudoephedrine meth. So I think that the Split izomer was successful except for the mass tragedy of only 11 grams. The problem was probably mainly that I had a bit of a problem during filtration with the fact that the funnel on the suction flask did not seal well and it might also help to wash off the tartrate salt during filtration, but please advise me how much water I can use for this so as not to disturb the solubility of the tartrate in water and thus did not get L isomers into the product. Well thank you

FringgRepeat the isomeric separation for a higher yield.

Freebase the failed salt and repeat process

- Wash it with cold anhydrous methanol, the L-meth/tartaric acid mixture is not soluble in methanol.

 

[Fringg]

Repeat the isomeric separation for a higher yield.

Freebase the failed salt and repeat process

- Wash it with cold anhydrous methanol, the L-meth/tartaric acid mixture is not soluble in methanol.

Acab1312Thanks, I'll try and let you know. Please, what temperature should methanol be, just put it in the fridge or should I use the freezer instead

 

[Acab1312]

I would recommend the freezer. In this case, the colder the better. The temperatures were never measured, I always store my methanol in the freezer.

-The polarity (polarimeter tested) after one pass

- H20 (68-73% d)

- Methanol (71-76% d)

- Rusznak process, toluene as a benzene substitute (still failed racemic)

- Pope - Peachey : h20/hydrochloric acid
(65-80 % d is time-dependent)

I prefer the method with h20 because of cost, time and simplicity.

I hope I could help.