but swim ran a 3g MeNH2/al/hg Osmium style yielding 2g of the hcl salt, 52%. not quite sure what's holding back the yields, maybe he balled the extra heavy duty foil too tight and dripped in all the ketone over 1h while not enough Al was exposed. it took all night for the foil to finish breaking down.
then swim ran a 4.1g MM reduction. timed it very nicely, 1h of ketone drip and 15 minutes later the Al was gone. basified with 43.3g NaOH in 50% aqueous solution. pH went up to 14 and sludge turned black (argh). 10% yield.
previous 1.6g MM reduction gave 41% yield, nothing special there.
so swim got some flashing, amalgamated 12.75g in 50ml MeOH, dripped in 96g of 15% nitro (14.4g MeNO2, about 77ml MeOH, some castor oil, no water added), let reflux 2h, added 15.7ml 50% NaOH, let reflux and stirred overnight. swim boiled it over trying to distil out of a flask 4/5 full (please, laugh...), switched to a bigger flask, and distilled 60ml of 4.6% MeNH2. sludge didn't swell up during gentle distillation.
so, abacus (love your synth, i really do) reduces 3mol of nitro and gets 1400ml of 6% MeNH2 ~= 2.2mol (disregarding the density of MeNH2 ), 73% yield. swim may have alot to learn, but at least he knows to add more MeNH2 than this to 178g of ketone... for 2.2mol MeNH2 use 130-156g ketone. pm me for details.
anyway, swim reduces .236mol nitro (undistilled 15%) and gets .0725mol, 31% yield.
so basically, swim recovered half the MeOH added origionally and got half the yield expected. any suggestions? add more MeOH to the sludge and distil again? use distilled 8% MeNO2 (doubling the solvent volume) next time? its probably the fukkin castor oil... bad shortcut.
anyway, closer to the origional topic, how do you gas 100+ grams of amine? it seems to me that dripping hydrochloric onto sulfuric, the sulfuric is going to get diluted and useless before enough gas is put out. so who prefers NaCl + sulfuric for gassing alot of product? or do you add pregassed IPA, then crash the salt with acetone (or ether)? last is probably the most idiot-proof large scale option if you weigh the IPA, determine HCl concentration, and add an exactly equimolar amount.