Ketone was dripped in over 5 minutes or so.I can't see how this could affect rx.Roundbottom adds it all at once.Raf used 80 grams of NaOH mixed with 240 mls of water.130 grams methylamine.HCl in 130 mls of water was used.About 700 mls of denat EtOH was used as solvent.NaOH solution was poured into MeAm.Cl solution and resulting methylamine freebase solution was added to rx mix before ketone.Otherwise followed RoundBottom Os/BB writeup.
https://www.thevespiary.org/rhodium/Rhodium/chemistry/redamin.os-bs.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/redamin.os-bs.html)
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, 2.8)
1133.2g 30% NaOH solution for basification
NaOH: 339.9g
dH2O: 793.2g