MDMA purity.

[wolfx]

I have a few questions on MDMA purity :
1) What would be the % content of MDMA vs. impurities in a typical street tablet ?
2) Same for Al-Hg, free base not distilled.
3) Same as 2, but with free base distillation.
4) Are any of the typical impurities psychoactive, can someone feel it when taking it ?
5) What is the brown impurity, that shows up in most methods, dissolves in acetone ?

[Rhodium]

1) Hopefully of high purity, but this can vary VERY much.
2) I'd guess around 85-90%. When Shulgin distills the crude freebase from an Al/Hg reductive amination, he gets a return of 75% (on a weight basis) of pure freebase. Some of the freebase is destroyed during distillation, because it will react with the impurities present in the crude freebase at the temperatures involved, so the crude freebase should be more than 75% pure if it was analyzed with a GC or similar.
3) If you collect the freebase in a narrow temperature interval (like five degrees) when distilling, the purity should exceed 99%.
4) It hasn't been determined scientifically, but I definitely believe that impurites present can cause side effects.
5) The brown impurities probably consists of various polymers of unknown composition.

https://www.rhodium.ws

[STQ]

There can be all kinds of impurities in street tabs - intentional and not.  Almost an infinite number of possibilities.

One thing that's pretty easy to carry over is a little MeNH2-HCl.  This will make your product stinky in the long run, so it's worth getting out.

If you want *pure* product, there's not need to distill the freebase, which is pretty lossy (although it does ensure that all the MeNH2 is gone).  Just do an A/B extraction sequence on the product and then gas out of toluene or ether.  The gassed product should then be recrystallized.  Any of a number of solvent systems will work, but I guarantee that nothing is easier than acetonitrile if you can get it.  Use 3.5-4.0 gm acetonitrile per gm of crude product (if it's decent) and you'll get fantastic white needles with no loss of good product.
STQ...

I can take it or leave it, but, so far, I always seem to take it...

[elfchemist]

typical street tablet

What is the difference between the tablet bought from the low level dealer and the ones you buy from the industrial scale MDMA operation in Holland? You know the one with the expensive pill press. Where do you think the tablets you drop come from? You can tell if the tablet is from a proper pill press by looking if it's out of shape, crumbling or soft...the tablets swim has found recently even have the indent line down the middle to make them easy to break in half....that's professional (not like the capsules STQ will be making), but it was bought in the street. Impurities in tablets are there from the start and not added  by the end street dealer. This is what was implied by using the term "street tablet".

The street dealer cannot afford and doesn't have the connections to buy a pill press and add their own impurities......So please people, don't bag out your local street dealer for impurities in your tablets.......
-eLF

[Osmium]

> If you want *pure* product, there's not need to distill
> the freebase, which is pretty lossy (although it does
> ensure that all the MeNH2 is gone).

With the right sized equipment these losses will be small. They were typically around 3% for me. I specifically remember a distillation of 42g freebase, and I ended up with almost 40g distillate.

> Just do an A/B extraction sequence on the product and then
> gas out of toluene or ether.

ALWAYS do this A/B. There are tendencies lately to leave out this simple step, apparently because some of the nitro writeups do not contain it. Bees taking such shortcuts deserve to end up with brown tarry peanut butter, it´s time they read PIHKAL again. There is NO excuse for taking shortcuts, and those not understanding this step aren´t ready yet for success.

[Quicksilver]

What is the difference between the tablet bought from the low level dealer and the ones you buy from the industrial scale MDMA operation in Holland? You know the one with the expensive pill press. That's making the assumption that the dealer hasn't bought high quality mdma powder and pressed it his/herself.

[wolfx]

I have evaporated out the MeOH, done the A/B, then decided not to try to distill it, instead crystalized from H2O and HCl. It had a lot of brown impurities, but after three acetone washes it became almost white. I got 67 capsules of 70 mg each. The high is clear, maybe just a bit more stoning at the beggining, I am not quite sure yet, but good enough for now. I want to improve my technique and to try again later on. I am taking a break now, but I will keep posting.
Thanks to everybody who contributed to this thread.
W.

[Osmium]

> I want to improve my technique and to try again later on.

Then don´t do that HCl/evap thing again. Shudder.
Your 5 grams of honey can easily be crystallised by gassing.

Add some salt to a small flexible PE bottle with attached plastic tubing, squirt in 2ml of conc. H2SO4, and then gas your honey with it by sticking the tubing into the solvent and slowly squeezing the bottle, bubbling the air/HCl mixture through your solvent.. Beware of suckback, take the tubing out before letting air back into the bottle. Repeat until your solvent is either full of crystals, or crystallisation stops. When HCl generation ceases add another 2ml of H2SO4. This is almost non-smelly, can be done in your kitchen with a little ventilation, and works perfectly. Method brought to my attention by Stoni (thanks honey).

[yellium]

Have said it before, many times: pre-gassed IPA or ether.

Nothing as annoying as having to much glassware around when doing the last step and fucking things up.

[spric]

OK, since the topic is mentioned, can anybee explain some nasty dreams of impurities.  Once upon a tyme, a large pile of nice white stuff, whose freebase was fractionally distilled, was quite wet with xylene, so it was spread to dry.  Days later, a busy bee went to check on the pile, well surprise!! it was fucking bright orange.  The solvent which was put to use in gassing was placed at ~-30C for a few days to shove out what was left, well, crystals formed, but they were a definate violet.  Some other purple stuff was nearby that resembled pine tar in its consistency?  What the fuck?  (performed by my friend's grandma in law 4 score and seven years ago using the wackathon followed by ye' old borohydride)
it's 4:20

[Rhodium]

Yellium: How much HCl can IPA and Et2O hold (concentration)? Will the alcoholic solution be stable for exteded periods of time, or do you risk isopropyl chloride being formed?

https://www.rhodium.ws

[wolfx]

To Osmium :
I have one 125 ml sep funnel, I have someone at a glassblowing store to adapt a 24/20 joint, so I could easily make a H2SO4/HCl gas generator. I have tried to gas it, the generator worked fine, plenty of HCl gas but no crystals. I have the folowing explanations :
1) I did not use a drying stage in the HCl generator, also I used 93% H2SO4.
2) The free base had lots of brown contaminants.
3) I used a just a bit of freebase in about 200 ml toluene when I tried it, maybe I needed also greater concentration. Can someone please give a good ratio ?
4) Your inputs are welcome.
I plan later on to distill the freebase, to add the drying stage in the HCl generator and to be more careful with H20,I hope then the crystals will show up.
By the way, I have a small problem pending with the freebase distillation, I plan another post just on this one later on.
Also, I think partial success on my second try is OK, I had by far more crashes when learning to grow mushrooms. Right now if I can fix the free base distillation I thing the remaining problems are more or less easy to fix.

[yellium]

According to acros, you can get 5-6 N solutions of HCl in IPA. It's good enough for X, where you add relatively large amounts of IPA. I've prepared a saturated solution of HCl/IPA and used it over a period of a year and never had any problems. I did switch over to ether/HCl because you can't add to much ether when you try to crystallize things out (if your solution is acidic enough).

[Osmium]

Wolfx, try the method I outlined above. I prefer it over the all-glassware HCl generator. It won´t break, it´s cheap, much easier to clean, less smelly and not suspicious to have.
I have successfully used this method in small and medium sized reactions, and with the proper amounts of NaCl and H2SO4 and the right-sized plastic bottle it should even be usable for mole-sized and bigger gassing jobs.

[wolfx]

First of all let me correct some typos :
1) I mean 24/40, not 24/20.
2) I think I mispelled "following".
3) I mean "think", not "thing".

Thanks Osmium, I think I will just let it stay like this, or will try to recrystalize from boiling IPA, but I think it is not so impure that justifies it, I think also I would loose too much product. By the way, I think more than half the freebase evaporated, you are right, this crystalization method is no good.
For me, I am done with this thread, unless you guys have something else to say.
Thanks to all.
W.