"MY" MDMA freebase crystallization

[Doubleboil]

I read a lot of different threads and posts asking and talking about MDMA freebase crystallization methods.
I guess many of them are tested and other ones are only taken from litherature.
I tested some of them and as always I post the most effective in my case and for what I need that dont means that is the BEST method only means that is the BEST one for ME.
Normally I dont like to post detailed methods as this one Im very cautios with them because people used to understand that Im posting the BEST and unique method with all the collateral consequencies that It has, I prefer to post complete and concrete synth not General methods.

Anyway here It is:

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

2. Heat the mixture gradually while stirring until 130C

3.Has ready a bucket, with 10 times the volume of initial freebase, of freezed acetone that has been at least 48 hours in freezer

4. When mixture is at 130C stop heating and pour It fast in the acetone bucket with vigorously stirring.

5. Leave the bucket in the Freezer at least 72 hours.

6. Take out the bucket and Filter solids with vacuum until It get dry, at the final part of that process pour a small amount freezed acetone over the solids to wash them before totally dry. The filtered acetone is keep It in the Freezer to try to crystallize more material if nothing else crystallized you can let the acetone dry at RT in a flat plate or similar to recover material or freebase

7. Once is completely dried Crush it and convert all into powder.

8. Solve the powder in distilled hot water(1gr/1ml).

9. When all the powder is solved Heat the mixture until 112C with some stirring and throw It fast into the cristallization bucket choosen.

10. Leave the bucket in a "calm" place, no Air flow, no movements, vibrations... At least 48 hours at RT after 48 hours put It 30 min in the Freezer before Filter It.

11. Filter the crystals and wash them with freezed acetone, the filtered liquid is saved to add It in the step 9 in the Next batch.

I Hope this method could solve most of crystallization issues that you could and the questions sent too.

I would like to clarify again that is not the BEST method or the unique one, Its just one more there are a lot of methods and techniques Im just posting the more appropiate for me, for my case and for my circumstances.

Thanks.

btcboss2022Hi. I want to ask. In step 2, is 130 degrees to evaporate water and traces of water?
after this heating, if left at Room temperature, theoretically would if crystallise? Just much slower?

 

[btcboss2022]

Hi. I want to ask. In step 2, is 130 degrees to evaporate water and traces of water?
after this heating, if left at Room temperature, theoretically would if crystallise? Just much slower?

DoubleboilIt will crystallize for sure the reason to do it in freeze acetone is to clean it, you only should avoid acetone step in the case that your freebase is completely pure(purified by steam distillation or vacuum distillation)

 

[Unreacted Freebase]

It will turn to a thick gummy mass almost like tree sap. it will turn to white crystal powder once you pour it in acetone.

 

[Doubleboil]

It will turn to a thick gummy mass almost like tree sap. it will turn to white crystal powder once you pour it in acetone.

Unreacted FreebaseI do have gummy mass right now. So heat it up and pour into cold acetone? White crystal powder should show immediately or after some time?

 

[btcboss2022]

I do have gummy mass right now. So heat it up and pour into cold acetone? White crystal powder should show immediately or after some time?

DoubleboilI think you have 2 options here:
- If this "mass" is totally clean you can wash it with acetone(keep the acetone) dry it and cristallize it with water.
- If not clean the best option is heated to 130C and pour it in freeze acetone while stirring vigorously crystal powder will appears while you stirring but you must keep it in the freezer anyway.

 

[Doubleboil]

I think you have 2 options here:
- If this "mass" is totally clean you can wash it with acetone(keep the acetone) dry it and cristallize it with water.
- If not clean the best option is heated to 130C and pour it in freeze acetone while stirring vigorously crystal powder will appears while you stirring but you must keep it in the freezer anyway.

btcboss2022@btcboss2022 thank you. Just to clarify. If I wash this sticky mass with acetone, it should be immiscible? Therefor use separatory funnel and wait for dry?

if poured to cold acetone, after stirring. How long to keep in freezer and should I be expecting a ice block like in your picture from another post?

 

[btcboss2022]

@btcboss2022 thank you. Just to clarify. If I wash this sticky mass with acetone, it should be immiscible? Therefor use separatory funnel and wait for dry?

if poured to cold acetone, after stirring. How long to keep in freezer and should I be expecting a ice block like in your picture from another post?

DoubleboilAll these details are here in that post read it please

 

[Unreacted Freebase]

@btcboss2022 thank you. Just to clarify. If I wash this sticky mass with acetone, it should be immiscible? Therefor use separatory funnel and wait for dry?

if poured to cold acetone, after stirring. How long to keep in freezer and should I be expecting a ice block like in your picture from another post?

DoubleboilIf you pour the acetone over the gummy mass it will harden and when agitated and broken up will be turn a fine crystalline white/grey tan powder depending on impurities which you can then Buchner and dry.

 

[Doubleboil]

@btcboss2022 One final question. This post says to ph till 3. And others say ph 6. Is there a pro and con to either or? Thanks.

 

[btcboss2022]

@btcboss2022 One final question. This post says to ph till 3. And others say ph 6. Is there a pro and con to either or? Thanks.

DoubleboilAt PH 3-4 you assure that all salt is precipitated in PH6 probably you will get crystals more oily than they should and more difficult to dry it. Anyway test it yourself as we all done bro too lazy I think hahaha

 

[Unreacted Freebase]

Correct. sometimes its as instant as super fast raising cake sometimes you need to give it a swirl and let it stand in the freezer. but generally it will appear very fast. looking almost like cottage cheese while wet.

 

[Doubleboil]

Correct. sometimes its as instant as super fast raising cake sometimes you need to give it a swirl and let it stand in the freezer. but generally it will appear very fast. looking almost like cottage cheese while wet.

Unreacted FreebaseAfter filtering. Waiting to dry. It’s looking more like wet white/tan powder right now. Not really “crystal” looking. I do know the next step is recrystallise with water.

 

[Doubleboil]

@btcboss2022 @Unreacted Freebase
I did the cold acetone. Left in freezer. precipitated and settled on bottom. Separated the solids. Left out drying but still very mushy. Does this look right ? Thanks.

 

[kharpa177]

@btcboss2022 @Unreacted Freebase
I did the cold acetone. Left in freezer. precipitated and settled on bottom. Separated the solids. Left out drying but still very mushy. Does this look right ? Thanks.

Doubleboildid you heat up your ph 3 acidified freebase and drop it in ice cold acetone..? was it ok after it dried?

 

[kharpa177]

@btcboss2022 @Unreacted Freebase
I did the cold acetone. Left in freezer. precipitated and settled on bottom. Separated the solids. Left out drying but still very mushy. Does this look right ? Thanks.

Doubleboildid you heat up your ph 3 acidified freebase and drop it in ice cold acetone..? was it ok after it dried?

 

[Unreacted Freebase]

Dry it and wash it. I would agree with btcboss. Better to go for lower PH and make sure all freebase is neutralized. then have unreacted freebase in product Use roughly 430ml 37% HCL per liter of distilled freebase.

 

[Mr Good Cat]

Dry it and wash it. I would agree with btcboss. Better to go for lower PH and make sure all freebase is neutralized. then have unreacted freebase in product Use roughly 430ml 37% HCL per liter of distilled freebase.

Unreacted FreebaseAre you sure about 430 ml?

1L of FB = 907 gr
907 gr = 6.08 mole
430 ml of 37% HCl = 5.16 mole.

 

[Mr Good Cat]

Dry it and wash it. I would agree with btcboss. Better to go for lower PH and make sure all freebase is neutralized. then have unreacted freebase in product Use roughly 430ml 37% HCL per liter of distilled freebase.

Unreacted FreebaseSorry, pal. I was talking about meth today, so wrong molecular weight was used. You are totally right!

1L of FB = 900 gr (roughly)
900 gr = 4.66 mole

 

[Mr Good Cat]

how many ml of hcl 37% would be used to acidify 1 liter of mdma freebase

kharpa177@Unreacted Freebase suggests to add HCl in proportions 1:1.1 (FB:HCl).
Me personally would go little less: 1:1.05

Let's study how to calculate. It is very simple:

First, you need to calculate how many moles are in 1L
Molar weight of MDMA FB is 193.25 gr.
FB density is 0.9gr/ml, that means 1L of FB is 900gr
1L of FB contains 900/193.25=4.66 moles.

Then you calculate necessary moles of HCL
4.66*1.05=4.89 moles of HCl.

Then you may find in internet a table that shows molarity (molar volume concentration) for different percentages, and 37% among them.
In your case it is 12.08 mol/L.

4.89/12.08=0.405ml

@Unreacted Freebase suggests little more - 430ml

 

[Mr Good Cat]

@Unreacted Freebase suggests to add HCl in proportions 1:1.1 (FB:HCl).
Me personally would go little less: 1:1.05

Let's study how to calculate. It is very simple:

First, you need to calculate how many moles are in 1L
Molar weight of MDMA FB is 193.25 gr.
FB density is 0.9gr/ml, that means 1L of FB is 900gr
1L of FB contains 900/193.25=4.66 moles.

Then you calculate necessary moles of HCL
4.66*1.05=4.89 moles of HCl.

Then you may find in internet a table that shows molarity (molar volume concentration) for different percentages, and 37% among them.
In your case it is 12.08 mol/L.

4.89/12.08=0.405ml

@Unreacted Freebase suggests little more - 430ml

Policja Polskafuck... shit...
not 0.405 ml, 405 ml of course!

 

[Lilred]

Dry it and wash it. I would agree with btcboss. Better to go for lower PH and make sure all freebase is neutralized. then have unreacted freebase in product Use roughly 430ml 37% HCL per liter of distilled freebase.

Unreacted FreebaseSo what is the perfect hcl addition exactly for 1L FB

 

[kharpa177]

So what is the perfect hcl addition exactly for 1L FB

Lilredhow many ml of hcl 37% would be used to acidify 1 liter of mdma freebase

 

[kharpa177]

how many ml of hcl 37% would be used to acidify 1 liter of mdma freebase???