Author Topic: Horrible yield after recrstyallization  (Read 2311 times)

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notta234

  • Guest
Horrible yield after recrstyallization
« on: November 09, 2004, 12:03:00 AM »
SWIM had about 38g of MDMA powder after completing gassing. SWIM took this 38g of powder, dissolved it in a minimal amount of boiling IPA (91% IPA dried 3x MgSO4). This was let to cool to room temp, and a healthy amount of dried acetone was added. This mix was then placed in an air tight container, and kept in the freezer overnight. After filtration, only 16g of powder remained! SWIM is planning on boiling down the IPA/acetone mix to recover as much of that crystal as possible, and then peform another recrystallization.

SWIM is curious if anybody has any idea why the hell he lost so much product? He has been very careful to follow all directions closely, A/B washes and whatnot, and has a hard time believing that there was 20g of crap mixed in with just a tiny amount of X. SWIM had used 36g of MDP2P, so he was expecting a much higher yield. He has done other reactions with appropriate pre-crstallization yields, but has always lost more than he though was correct during recrystallization... but this >%50 loss is bullshit!!

Any suggestions on different methods would be highly appreciated.

Thanks

amine

  • Guest
Use anhydrous IPA, you can buy it at allĀ ...
« Reply #1 on: November 09, 2004, 08:10:00 AM »
Use anhydrous IPA, you can buy it at all electronic stores, its used for cleaning boards, no problem OTC. Honestly, I use just straight IPA and my yields are always good.

Do your boiling or just leave the IPA out to evaporate, it'll only take a day or two.


fnord

  • Guest
evap
« Reply #2 on: November 09, 2004, 05:37:00 PM »
evap the ipa some before you try to filter it and you might get a better yield,how souluble is mdma in ipa/acetone?or evap completly and listen to amines idea


Xaja

  • Guest
Hey
« Reply #3 on: November 10, 2004, 04:09:00 AM »

but has always lost more than he though was correct during recrystallization...




Two possibilities:

1) A lot of your 'product' was not MDMA. You need to distill or otherwise clean up more before attempting a recrystallization.

2) You are doing it wrong i.e. using the wrong ratio of solvents or the wrong solvents. Check you have these correct, and do some reading on recrystallization techniques in a chem manual of some sort, then come back and UTFSE to apply it to MDMA.

Happy gassing!  8)




indole_amine

  • Guest
hm..
« Reply #4 on: November 11, 2004, 05:17:00 PM »
Boil away some of your IPA/acetone solvent mixture; do so until a slight cloudiness set in. Now add a squirt of anhydrous acetone, and place in the deep freezer for some hours (or maybe 1-2 days?). More crystals will form.

This is usually called "concentrating the mother liquor" and normally is part of the standard recrystallization procedures...


indole_amine