"MY" MDMA freebase crystallization

[Davidrobinson]

It should be ok because you crashed ot out in acetone. More acid just makes more impurities.
Did you get big crystals from pouring the hot acidified freebase into cold acetone?

 

[btcboss2022]

When I did It in past at 120C yes I got Big crystals now at 130C I get shiny powder

Thanks.

 

[kharpa177]

I adjusted the freebase to ph3 and heated it up, I added a little cold acetone and these crystals were born... I added 4 times more acetone and put it in the freezer

 

[kharpa177]

this is correct after I put acetone the solution turns white

 

[btcboss2022]

I Guess thats not the my way then.If you are asking me about issues with a different process you should explain the previous steps.

 

[kharpa177]

A Photo Essay on the Nitromethane Al/Hg

I made this synthesis only at the end that I crystallized in the way you said

 

[kharpa177]

.

 

[kharpa177]

 

[FredDurst]

Hi mate. I have a few questions about this part of your procedure

Do you leave the mixture at 112c until water boils away or just get to that temp and pour straight in the bucket?

In the bucket you have cold acetone again?

Do you not loose loads of product in the remaining water?

Thanks

 

[Mr Good Cat]

Last time, when re-crystallizing dry salt with this 108C method I lost 5.4% of dry weight.

 

[Mr Good Cat]

Sorry, I forgot to count the leftovers from acetone. So, it is much less: 2.6% lost, that's not bad at all.

 

[kharpa177]

there are so many methods that even people are confused... I used this method and it doesn't work... some say crystallization at room temperature with cold acetone... others say it's by heating

 

[Mr Good Cat]

I don't doubt this method works. Even now I have just finished this method applied to the purified by ether freebase, and it works. The crystals are white and perfect. So I don't think I did anything wrong. Rather, something was wrong with the solution I received from you - the volume of contaminants was huge and even difficult to clean with ether.

For me the process itself is simple and completely understandable. I use a simple hotplate that can control the temperature inside the solution up to 102C, that take for me around 1 hour to warm 1:1 solution up to this condition. Then I change the mode finish it up to 108C controlling the plate temperature between 160 and 170C. This step takes around 30 minutes more. 90 minutes in total, that's it.

 

[bblanco]

I come exactly to this same matt powder. tooth paste and after drying this...i tried to re crystalise with water when i payed attention... no crystals... couple of days ago did three test the same time... couldnt remember what i did but all of a sudden in one bottle i had 5gr rocks white big crystals.... fucking hell ]cant remember how i did it..

 

[Mr Good Cat]

I guess, this method could be simplified if applied to the purified freebase as below.



1. Add portionwise cold HCL37% to the MDMA freebase (previously cooled too) while stirring until PH 3.


2. At this point we used 95ml of 36% HCl (that contains 65 ml of water) for 1 mole of freebase. Some of water will be evaporated be the heat released with reaction. But, probably, if we finish the acidification in 15 minutes (not in 30 minutes as I did last time when got white dry powder at the end of reaction) there will be approximately 40 ml of water for 1 mole.


3. Heat the mixture gradually while stirring until 108C with some stirring and throw It fast into the cristallization bucket choosen.

...


We simply skip preliminary crystallization as unnecessary step as the freebase is already clean.

 

[rothschild33]

how's the end result if you use undistilled MDMA freebase?

 

[Mr Good Cat]

I didn't try unfortunately. Last time I did the mistake while acidifying the freebase - elongated the process in time. So, as I finished it there was almost dry powder in the beaker. Then I sucessfully dissolved it and re-crystallized by heating up to 108C. Completely satisfied with the result.


But I guess, it shall work if some water still left after acidification.

 

[Mr Good Cat]

I mean, I had strong intention to try this "simplified" crystallization method while acidifying my "distilled" freebase last time, but did the mistake with timing. So I had to dissolve the salt 1:1 and recrystallize it by heating up to 108C. The result is perfect as expected.
Logically, this "simplified" one step crystallization shall be perfect if applied for "distilled" freebase. But, obviously it is not the way for undistilled freebase - huge level of pollutants presents, and it won't be purified by one time crystallization..

 

[bitcoinup2020]

Can I crystallize undistilled MDMA Freebase?

 

[kharpa177]

I crystallized the cold freebase with acetone and cold hcl is this correct?

 

[kharpa177]

I crystallized the cold freebase with acetone and cold hcl is this correct?

 

[Mr Good Cat]

everything is correct

 

[kharpa177]

1photo .. hcl gas
2 phot acidifier with hcl plus cold acetone in the free base

Is it normal after hcl gas for the solution to be cloudy? What do I do next?

 

[Unreacted Freebase]

cooking at higher temp 130c vs 110c for longer insures more water is lost.
The dryer the solution the faster the product will precipitate (faster also means smaller crystal size)
In order to grow the bigger crystal it helps to have some water content. It allows the product to dissolve and then slowly precipitate using the freezing technique.