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All 7 posts Subject: Horrible yield after recrstyallization Please login to post Down

notta234
(Stranger)
11-08-04 23:03
No 540503
      Horrible yield after recrstyallization

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
(Hive Bee)
11-09-04 07:10
No 540603
      Use anhydrous IPA, you can buy it at all ...

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
(Hive Bee)
11-09-04 16:37
No 540663
User Picture       evap

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

fume hoods are for pussys

Xaja
(Hive Bee)
11-10-04 03:09
No 540735
User Picture       Hey

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! cool

**FriedPiper**

I love BUSH! The pussy, not the President!!

indole_amine
(Hive Bee)
11-11-04 16:17
No 541039
User Picture       hm..

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}

homeslice
(Hive Bee)
11-12-04 18:02
No 541262
User Picture       correct ratio

What is the correct ratio of solvents if the ipa and acetone is used?
I saw on rhodium's one post that 7ml/g acetonitrile is used or a minimum of ipa. How much is a minimum? The same ammount?
Post 454897 (Rhodium: "Recrystallization of MDMA.HCl for Purity", Methods Discourse)

"Drugs and akahol have ruiinnned my life..." -Tyrone Biggums

MakoEyes
(Stranger)
11-13-04 06:16
No 541341
      well thats what recrstyallization is for...

well thats what recrstyallization is for... removing impurities, tho that does seem a bit low of a yeild... boil it down. hope you recover well, of course what you do recover will be damn dirty. Maby try purchasing ahydronus IPA instead of drying the watered down stuff. MDMA HCl is a bitch about water.

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	All 7 posts		Subject: Horrible yield after recrstyallization		Please login to post		Down


		notta234 (Stranger) 11-08-04 23:03 No 540503				Horrible yield after recrstyallization
						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 (Hive Bee) 11-09-04 07:10 No 540603				Use anhydrous IPA, you can buy it at all ...
						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 (Hive Bee) 11-09-04 16:37 No 540663				evap
						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 fume hoods are for pussys



		Xaja (Hive Bee) 11-10-04 03:09 No 540735				Hey
						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! FriedPiper I love BUSH! The pussy, not the President!!



		indole_amine (Hive Bee) 11-11-04 16:17 No 541039				hm..
						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}



		homeslice (Hive Bee) 11-12-04 18:02 No 541262				correct ratio
						What is the correct ratio of solvents if the ipa and acetone is used? I saw on rhodium's one post that 7ml/g acetonitrile is used or a minimum of ipa. How much is a minimum? The same ammount? Post 454897 (Rhodium: "Recrystallization of MDMA.HCl for Purity", Methods Discourse) "Drugs and akahol have ruiinnned my life..." -Tyrone Biggums



		MakoEyes (Stranger) 11-13-04 06:16 No 541341				well thats what recrstyallization is for...
						well thats what recrstyallization is for... removing impurities, tho that does seem a bit low of a yeild... boil it down. hope you recover well, of course what you do recover will be damn dirty. Maby try purchasing ahydronus IPA instead of drying the watered down stuff. MDMA HCl is a bitch about water.

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