03-16-04 13:26
No 495559
Okay where to begin???
SWIM took about 30g of P2P and did a Al/Hg reductive amination.
Mistake number 1... about 15 mins into the reaction he noticed the condensers were getting hot. Oh no. The fucking water pump came unpluged. The top of the condensor was about 100F and he pluged it back in and continued.
He finished that up added the NaOH solution and everything was going okay (he thought). He extracted with 500ml, then 250ml, then 100ml of xylene.
The xylene + honey had a yellow piss color to it.
Mistake number 2...
He dried the solution with about 30g MgSO4 and went to filter when, oh shit, a hole in filter and its the last one. He thinks about 5g or so got back into the solution. Anxious to yield something he decided to gas while the MgSO4 was still present.
So, he gassed and gassed and the only thing this did was gave the solution a nice little pink tint (water). Still nothing. Time to sleep and get some filters.
He got some filters, filtered the solution (maybe some honey is in the filter cake, he'll give it a taste test later). Solution still has a pH about 1. So he distilled. It got the pink color out, back to piss yellow. He distilled off about another 200ml just to be sure. Removed the heat and... OH MY GOD!!! What is that? Finally white crystals were salting out of the solution!!! Thank god!!! He chilled in the freezer and filtered out about 6g dry, snowy white Honey-HCl.
The light is appearing at the end of the tunnel.
He gassed again (he didnt check the pH before starting the gas) and... nothing. Still piss yellow.
Well, the distillation worked before so he tried it again, but this time nothing happened when it cooled. His heart sank.
At this point he decided to get a professional opinion. Anyone? Should he try to basify the solution? Distill some more? Do an ancient voodoo anti-water dance? Is that all he is getting because of the water pump coming unplugged? He is clueless and going through an emotional breakdown. Help.
(Wonderful Personality)
03-17-04 06:02
No 495715
You have:
- some pep in the MgSO4 which you filtered out after gassing
- perhaps some pep in the gasses xylene
Evaporate the xylene and dissolve and recrystallize whats left back from hot IPA/acetone.
Dry the MgSO4/pep which you filtered out and extract this with three portions of HOT IPA, then boil most IPA away and add acetone to crash the pep out. MgSO4 will not dissolve in IPA, pep will.
Then try everything again - there isnt more pep to find in the leftovers you probably have lost lots during the Al/Hg anyways. But you have got something on your first try and thats more than many can claim here. Me included.
