01-27-04 18:02
No 485012
Ok SWIM wants to know where 200g of product just went?
Ran a bunch (9) of Al/Hg, washed 5x with dH2O each 2x brine, A/B distilled freebase and gassed and WOW all kinds of salt falls out of solution, filtered <Was doing the gassing in 3 different bottles.> everything was going fine, a after a 3rd trip to gassing started to go slightly orange <Figured there was a little H2O in the gassing near the end>
Everything was left to dry and weighed still a little wet ~400g, Okay decided to recrystallize, split into 2 4L beakers, brought 1.5L of acetonitrile, brought to boil and added it to the ˝ the MDMA.HCL, slowly added acetone, let everything cool and recovered crystals –BUT- the crystals had a tinge of brown to the crystals, where did that come from? And after recovering all the crystals there was only 89g!! Where is the rest? Why did SWIM get brown crystals? I have used TFSE and SWIM can’t see why this would have happened…
This is the 5th dream SWIM has had and this is by far the worst! <Feel like SWIM should have never recrystallized, should just have washed with acetone and left it at that.>
(Hive Bee)
01-27-04 21:12
No 485050
how did you prepare your md-p2p?
If it helps I've encountered yellow/tan/brownish product only when using the performic acid method to make my md-p2p. The product was fine in all cases and still recived rave reviews. Then again I've never used the Hg/Al method to put on the bussiness end so this may deserve some thought......
Bigamy is having one wife too many. Monogamy is the same."
-- Oscar Wilde
(Hive Bee)
01-28-04 03:10
No 485067
Well....the 'rest' is obviously still in solution! Here are a couple of suggestions (in order of preference):
1) Remove solvent by rotary evaporation then do a 'proper' slow recrystalization.
2) Add a huge excess of acetone, filter the resulting mess and do a 'proper' slow recryst
What i refer to a 'proper' recryst is as follows:
Place residue in a 1L RB flask with enough MeCN to just cover. Add a reflux condensor and bring to ~100C. Add MeCN in 10ml portions, and allow to come back to reflux before adding more. Stop addition when solid is all in solution. Reflux for another couple of minutes and then stop heating.
At this point i would allow it to return to RT slowly. Then, leave it uncovered overnight and the next morning you SHOULD see nice fluffy white product. If not, then add acetone dropwise until you see lasting turbidity, and refrigerate for a few hours. If you still see nothing. Then add slightly more acetone and repeat.
When it comes to recrystalization, patience and good technique are very important in producing nice pure product.
Fan of shulgin
Peace, love and empathy
(Hive Bee)
01-29-04 13:42
No 485359
I used acetonitrile to recrystalize 2 different times and It made no differnce in the color in my side of the world. I never messed with it again. You have to make sure that your crystals are completely dry b4 recrystalizing because just a trace of water can hold back 50% of your supposedly recrystalized product.