"MY" MDMA freebase crystallization

[Doubleboil]

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?

 

[btcboss2022]

It 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]

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?

 

[btcboss2022]

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.

 

[Doubleboil]

@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]

All these details are here in that post read it please

 

[Unreacted Freebase]

If 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]

At 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]

After 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]

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

 

[kharpa177]

did 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]

Are 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]

Sorry, 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]

@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]

fuck... shit...
not 0.405 ml, 405 ml of course!

 

[Lilred]

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

 

[kharpa177]

how 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???