swim dreamed his first successful performic oxidation of safrole last night.
18.3g safrole was distilled at 140-144C, +KOH, 15.1g isosafrole at 150-158C.
swim used labtop's modified performic from the sticky thread...
he reduced the amount of bicarb proportionally, but used the slight excess of performic intended for 16.3g iso. mixed 1h, added to 46ml dcm, iso, buffer which did reflux nicely after 1/3 the performic was in.
seperated dcm, extracted with 10ml more, directly stripped as much dcm as possible first at atmospheric then aspirator vacuum yielding 21.8g glycol/monoformyl glycol. looks good so far...
heated with 30ml methanol, added hot 15% h2so4, refluxed slightly for 2h.
dark heavy oil falls out
, tapped, extracted with 2x 20ml 1x 10ml dcm.
well, labtop doesn't mention washing, but bees say to neutralize after h2so4-
so swim washed 3x 20ml dH2O, 3x 30ml 5% NaOH. the first NaOH wash was very dark, the next 2 were brownish, though they would help.
washed 2x 20ml saturated NaCl solution. dried over (too much) 12.9g MgSO4.
thing is, after gravity filtering the MgSO4 (who knows why), swim only had 25ml DCM left of the 50ml + ketone before washing. there were really no emulsions to speak of, the NaCl wash seperated slowest so swim cursed, and washed the MgSO4 with some more fresh DCM.
he distilled it with an un-packed claisen as a column, got a nice little iso forerun, and just ba-a-arely pulled 5g suspected ketone at 180C.
so swim wants to know, where's that other 5-10g ketone hiding at?
in the washes with dcm, or did that evaporate? eh? where is 'dat shit at?
swim supposes he should weigh the shit that didn't distill... feels like a newbee
. too bad 1oz of sassy is gone so quick. coming up... Leuckart!