SWIM carried out seperate experiments to explore this idea of using alcohol.
Experiment 1. Usual method as done many times1 mole hex
4 moles HCL in 32% solution
NO addition of NH4CL, not needed in my opinion (I agree with placebo on that)
100mls water (to stop solution being saturated)
Reaction time of 6 hours at 100DegC (water bath).
Reduced to half volume by atmospheric distillation and cooled (vogel workup, except vac not used).
NH4CL that precipitated was filtered.
Liquid again distilled until 160DegC mother liquid temp
Cooled, which formed a solid.
Solid crushed up and vac filtered, washed with ice cold ethanol, acetone and recovered methylamine.hcl dried
Filtrate again heated, cooled, and crystals collected.
Finally left with a concentrated syryp that refuses to crystalise which, correct me if i'm wrong, Vogel states as being mostly trimethylamine
So, recovered colourless methylamine.hcl (with insigificant impurities IMHO) that dissolves completely in cold alcohol. EDIT, I mean room temp methanol, and hot ethanol.
Yields range from 60-80% w/w based on starting hexamine.
Experiment 2. Same as above, except with the additon of ethanol1 mole hex
4 moles HCL in 32% w/w solution
NO extra NH4CL added
3 moles ethanol
100mls water
Heated to reflux for a couple hours (bath temp around 75DegC), then the formed ethyl formate was distilled out. Once that had stopped, heated to around 100DegC for another 4 hours.
Then exact same work up as previous experiment
Yield of dried methylamine.hcl ( as opposed to the product contained in Orgys picture in this thread) was 55% w/w based on starting hex
ConclusionAdding ethanol made temp control easier.
Less gas, slower reaction, but somewhat more pleasent.
Yield was if anything worse, following the vogel type workup as normally done, and written, by SWIM
Last pointDo you think it's possible that some bees doing IPA extractions, simply boil the IPA away and then claim that the hardened mass is their yield. Whereas others then crush up said solid, filter, wash and dry?? which would explain some discrepancies IMO.
Abacus