hi,
swim made a LAH (14,5g) reaction with P2NP (20g) in THF...
- refluxed 6 h
- quenched
- distilled off the THF in vacu
- yellowish residue with fishy smell received
and this is the point where the disaster starts:
- poured 200ml water to this residue gave me a nice
golden layer on top of milky water
- this was actived with HCL to pH 1
- washed 3 x with DCM, which removed most of the yellow
colour
- made basic with NaOH to pH 12-13 and at this point it
seems to be that the FB was the bottom layer, hm?
- anyway, the FB was extracted with DCM. after evaporation
of the dried DCM, a light yellowish residue with
fishy smell received.
- made the salt of this with H2SO4 in ether/ethanol
BUT THIS WAS SHIT AT ITS BEST (no effects, no fun....)
swim made several LAH reactions before and the result was O.K. everytime (tried not to perform an A/B to make purer product).
but today swim tried to make better product, so he decided to make this fucking A/B.
can/t understand where the mistake is, also can`t understand why the FB before the AB is ON TOP of the water and after the A/B it was on the bottom of the water?
is it nescessary to do this a/b ? why not dissolve the risidue (after DCM evap.) in ether, drop in diluted H2SO4 and filter off the salt?
hope there is somebody out there, need help
thx