05-12-02 15:56
No 307746
Anyone ever use denatured ethanol for purifying mdma?
(Pioneer Researcher)
05-12-02 16:20
No 307756
It will dissolve a lot of product. You should dissolve the product in the minimum amount of alcohol, then add chilled 4 volumes or more of ether or acetone. I think IPA is better.
(Hive Bee)
05-12-02 18:25
No 307776
Are you saying you prefer the ipa over the ethanol or are you saying you prefer the ipa over the ether or acetone?
(Hive Addict)
05-12-02 19:13
No 307793
To recrystallize, you need a solvent that is somewhat or partially miscible with the MDMA. When the solvent is hot, it usually will allow more MDMA to become soluble. Then when the solvent cools, it can no longer hold the MDMA in solution, so it crashes out. IPA which is free of any water, or anhydrous, will work better than ethanol because it isn't as miscible with MDMA, so less product will be trapped in the IPA as it cools.
Sunlight mentioned acetone in conjuntion with ethanol to help reduce the solubility of the MDMA in the ethanol. Acetone is insoluble with MDMA, but soluble with ethanol. So the acetone will help push the MDMA out of the ethanol as it cools.
Mastery is based on the understanding and practice of technique.
(Hive Addict)
05-12-02 22:21
No 307843
IPA is a good cheap choice.
Anyone ever had success recrystallizing with hexanes? (weird choice eh?! but I believe it works!!!)
(Stranger)
05-14-02 20:48
No 308650
So far someone I didn't know has done the BS synth 3 times and after the Al/Hg step was complete. He took as much of the oil as possible with the Alcohol washes and just poured it all in a dish to evaporate ( I know, its not in the steps) Did the acid base thing to obtain the desired molecule and when the solution was basified the product fell out of solution. He collected it with DCM and poured it out in a dish to evaporate and it was allready in crystal form.????? Then washed with acetone. Why must he recrystalize? Was he wrong? It most certainly was very good. I guess my question is, why redo if its allready done?
DeJay
(Newbee)
05-15-02 03:29
No 308739
Dada, are you telling me you basified the solution causing the MDMA base to fall out of solution and form a liquid/oil which you then extracted into DCM???? WHat was the pH?
Upon removing the DCM why did you find crystals?????? when all you should have found was freebase!!!
If you washed this in acetone, you washed your goods away!!!!!!
Are you sure your not full of crap????
Abacus
(Stranger)
05-15-02 16:36
No 308976
Sidk followed the synth just as it says Now, slowly add 50mL of 25% NaOH solution to the aqueous layer. When you
do this the Aqueous layer will turn a milky white and may heat up just a
little bit. Not to worry.... A light brown oil will fall out of the
solution. This is your product (in the freebase form). Before collecting
it, wash the 'now basic' Aqueous layer with ~50mL of DCM. Shake and let it
settle out. Pour off the top Aqueous layer, and KEEP THE DCM THIS TIME!!!!
The DCM washes CONTAIN THE GOODS!!! Wash the aqueous layer twice more with
50mL of DCM. Combine those DCM washes that contain your product, and
continue.
At that point when these brown crystals fell out he did not want to distill so he just let it evaporate when he noticed he allready had crystals. So he hit these with acetone a few times. The mdma will not melt away but a lot of the brown did.(not full of crap) He then tested these (after drying of course) and believe me they were very good. I'm no chemist but I do know good x when I feel it. He has done the recrystillization but just wants to know why.
DeJay is not a liar. Thank you very much.
(Hive Bee)
05-15-02 17:04
No 308985
I got the milky white appearance upon basification and I also got a light brown precipitate. Now this precipitate did not have the appearance of oil because it sort of stuck together to inself and formed clumps. The precipitate/oil would not disolve in DCM so I thought it was not the stuff I was looking for. However, I left it in with the dcm extracts I got from the basified aqueous soln. and then did the bright star crystallization and got some some brown goop but no crystals. Over $2000 invested and hundreds of hours of research and work and brown goop.
Well----I had all that fun and learned/relearned alot of chemistry so its not a total waste. I'm going to disolve my brown goop in toluene and add some Mg. sulphate to dry it and then try the hcl generator. With the bright star crystallization there were too many things that could go wrong like not getting all the H2O out of the IPA.
(Title on BackOrder)
05-15-02 18:29
No 309036
take that brown goop, dissolve it in toluene, acidify it and extract your product with water, and then basify that water and extract your freebase with a nonpolar solvent.
(Hive Bee)
05-15-02 20:04
No 309108
Yes---I think you're right.
I'll try the a/b process and post the results.
(Stranger)
05-15-02 21:15
No 309156
Thanks Mr.DiM I thought I was going nuts. I wish someone (BS) could help on this. Here's what I think happened. Swidk thought it would be ok to spring for 99.9% Alcohol and used this instead of the 70% stuff and forgot to dilute when performing the AL/Hg and maybe there was just enough water produced by the Amine thingy going on (as you can see he's no chemist but he has read that water is produced in th rxn and he knows Methalamine will suck it up) that maybe it all got used up and when he did the extraction out of the rxn he used the same 99.9 stuff and there was just no water to allow it to be in oil form. He tried to crystalize anyway and pucked it up the first time. Not knowing any better he started over only this time he thought his vacuum was to blame so he just let it evaporate (laymans distill) when the goop dried he noticed it already looked like crystals. Washed it with acetone and VWALA crystals. He was felling a little bold that day and decided to chance about 50mg or so and wow. He was ranting someones name all night long. (Thanks BS) Although he did only come up with 12g. He was quite happy the rest of the summer and did definately have a pleasant spring.
DeJay
(Stoni's sexual toy)
05-16-02 00:05
No 309235
Sounds like you got the carbonate salt.
I'm not fat just horizontally disproportionate.
(Hive Bee)
05-16-02 01:50
No 309278
I have had the brown goop drying in petri dishes for a week now and NO crystals.
I did a bio-assay on the goop and had not one twinge of any kind of euphoria.
Sure, I'll do the a/b on it just for the experience but I don't expect much.
(Stranger)
05-16-02 18:02
No 309671
Someone I didn't know wonders what you mean by that Osmium.
Except for the recrystalizing step. He followed the synth just as written (except the 99.9% alcohol) Would the Carbonate salt of MDMA be easy to digest or something? less stabe?( it lasted more than a 9 months) a good thing? a bad thing? He thought it was very good allthough he noticed his dosage was better around 150mg. and wondered if it was just his personal preferance or that the x was not as strong. He has been looking for the same dream again but finds he can no longer duplicate it. After 3 attemps he only gets oil and thought he had messed up again because the first 3 had all gone as mentioned above. (I"m so embarrased
)If so, I have a question. How long can the suspect oil be held in suspense? As he has never completed his washes of the al?hg step and still has a considrable quantity left in a jar. (never throw anything away till your absolutely sure its no good[i read that somewhere]}
thanks for any help.
DeJay
(Newbee)
05-16-02 23:15
No 309814
Dada and Dimethyl, you guys really dont know what you are doing do you??? The answer is everywhere just read the sticky posts!!!!!!!!Read and keep reading until you get it
You will see the easiest thing to do post reaction is this.
1. Basify the al sludge with NaOH and extract the amine into toluene or xylene. Now you have freebase dissolved in the non polar solvent. Do you know what they are???
2. Seperate and extract into HCL solution. Now your amine is dissolved in the hcl and water which you then seperate from your non polar solvent (eg toluene).
3. Basify with NaOH so that the freebase precipitates out, hopefully as an oil that drops to the bottom of your seperating funnel.
If your not really fussy about quality then dissolve the freebase in clean toluene and gas with hcl.
All you have done is basify and evaporate the solvent. How can you have converted it to any salt???.
Your base must be reacted with hydrogen chloride eg HCL gas so that it forms the hydrochloride salt which is the crystals you want, not some mushy freebase which is probably all you have.
If you have some freebase lying around, dissolve it in toluene and gas it, your crystals (if you have any) will precipitate out.
Dada, you stuffed up by not following BS's write up to the end. That included making the hydrochloride salt, albeit a different method than gassing.
(irritable and cranky)
05-17-02 03:27
No 309880
It's funny to see some of the MDMA bees haven't got the principles of A/Bing down yet. You should hang out in the Meth forum a little, that's about all you see in there.
Back on topic, if you really want to purify by crystallisation, why force the crystals out so rapidly with dual solvent systems? Just dissolve in the least amount of hot alcohol/methanol/IPA that it takes to dissolve product and leave out somewhere to evap slowly. Then do a cold, dry acetone wash. Patience is a virtue, and you will be surprised at the difference.
Bored...
(Stranger)
05-17-02 21:24
No 310238
He(swim) thinks he understand the a/b washes.(duh) He has had 3 sucessful runs. He was only trying to understand HOW he got crystals as he had nevr done this before in his fucking life, with little more than a writeup to go by. NO he is not a (chemist) but I was kinda proud of him anyway. He DID do the rest of the steps on some and it seemed to mess it up. He didn't know why.(ph likely was off)
Well, he did and has been reading a lot for the past 3 years. He just doesn't post very often. Something a lot more people should try, obviously.(don't take that wrong) I know, a why the hell didn't you get oil instead of crystals search. Obviously it's over in the Meth section. How stupid of me.
The paticular step said " a light brown precipitate will fall out" and it was indeed that but only it was allready in a crystal form, hence the confusion. He tasted and liked it , what the hell. He wasn't sad about it. It's no big deal. What ta fu
I think from what I'm reading here though is Mr . M's wasn't good . I'm not sure but swims was. so he thought it was a good thing. Your right, he doesn't know.
I like the sound of the chilled acetone thing. Nice and slow. (saw that from a search he did)
He did have sucess with BS recrystaisation and it Was quick,as you said. And he did notice that no matter how many acetone washes it never came any purer ( a slightly yellowish or light brownish)
He does not use hcl and gas and all that because it's not in the BS synth. and that is the only reason other than availibility reasons and all that. It's simple, only make sure there is absolutely no water in the mix or you get crapola as they say.
DeJay