i didn't notice that you were following my writeup until this post.
SWIM just did a 900mmol (160.2g ketone) version; everything was the exact same reagents as the last 300mmol (53.4g ketone -> 50.6g salt [yes, A/B'd and recrystalized in IPA]). the results aren't fully dry yet, but the bulk is already dry and over 140g (same, A/B'd and IPA recrystal) with some still to be checked.
in this reaction, the ketone
was dripped in over 40m (not 100% certain of the addition time but thereabouts.) it did run slower and a bit cooler than adding it all at once. also, a new fredrichs condenser (as opposed to a 6 bulb allihn) was used this time.
ketone: 160.2g (900mmol)
MeAmCl: 182.3g (2700mmol, 3x excess)
dH2O: 182.3g
25% NaOH solution for MeAm liberation
NaOH: 108.0g (2700mmol, 3x excess)
dH2O: 324.0g
MeOH: 996.7g
HgCl2: 300mg
Al: 68g (2520 mmol, 2.
1133.2g 30% NaOH solution for basification
NaOH: 339.9g
dH2O: 793.2g