Swim used ketone and followed:(1/2 batch)
Procedure
Mixed 66.8g MeAm with 67mL H2O. Mixed 39.6g NaOH with 119g (119mL) H2O, and cooled in ice bath.
Set up equipment (1l rbf+condenser on top), started cooling, added stir bar. Put 26.7g Al foil in RBF. Added most of the 420mL MeOH to the RBF, saving about 50mL to wash out the ketone container. About 140mg of HgCl2 was then added to the RBF and the whole flask was swirled to mix the HgCl2 into the MeOH. Once the MeOH started bubbling , the cool NaOH solution was slowly poured into the MeAm solution. The smell of MeAm gas was now very strong. The basified MeAm solution, and the 53.4g ketone were then poured into the RBF. The remaining MeOH was swirled in the ketone flask and added to the RBF, and the whole flask was swirled a few times to mix everything. This reaction is nowhere near as exothermic as a Methyl Man Al/Hg Nitromethane. Stirring was attempted, but meybe your bar would not move, probably due to the Al foil weighing it down. During the reflux the solution was bubbling quite well, but was still diligently swirled a couple times every five minutes (if stirbar will not work). After the reflux subsided, the flask was swirled approximately every 15 minutes. When a top layer of clear fluid started forming, that means it's time to swirl. The temperature rose quickly to about 72°C with lots of foil floating on the top, and lots of bubbles were evolving, but it stayed in control (if using thick foil, you may need some heat to kickin the reaction). This is with all the ketone added at once. The reaction was left to run for 4.5 hours, and began to calm down after about 45 minutes from the addition of the ketone. When it calms down a bit, prepare the basification solution (230g 85% KOH added to 469mL dH2O) to give it time to cool. Heat was added to the RBF after about 75 minutes to get the temperature up to about 65°C. Once the reaction is deemed finished, (there isn't really an indicator to look for, just when enough time has elapsed) strain/filter out any unreacted foil chunks. The foil in the strainer was rinsed with about 50mL H2O which was added to the reaction contents in a 2L beaker. The mixture was slowly basified by pouring the KOH solution into reaction contents, and was stirred on a stirrer for about 10 minutes. Some bubbling was observed as any remaining foil was reduced. The mixture was extracted with 1x 500mL, 1x 200mL fresh toluene by pouring the toluene into the beaker and continuing stirring. After separating the extractions were combined. The toluene started out clear, water-white, and after the extractions was slightly cloudy and slightly coloured. The combined toluene extracts were washed with 3x 700mL dH2O, 1x 700mL brine (saturated NaCl). Most of the cloudiness cleared up after the washes. (I do an A/B here but some exclude it)The toluene was dried in 40g dried MgSO4 for 10 minutes. The toluene was then gassed, and filtered 4 times. Even though the crystals were as white as has been ever seen, the crystals were put into some boiling acetone and filtered again. Total yield after acetone cleaning: 92.4% (w/w)!!!
not sure who wrote it but you the man!
After gassing swim ended up with 18.3g of white crystal
& 3.1g of less white crystal.
total 21.4g
Swim will wash crystals in hot acteone.
Thx u Methlab bee who shared this info with swim
