roughly how long should the aluminum reduction take in a ~100g scale Osmium MeAm Al/Hg?
after the initial reaction with HgCl2 and then the MeAm/NaOH mixture, the reaction slowed way down. the Al doesn't seem to have gotten much smaller (but it's probably thinner) after about 12h of stirring. the solution is now dark grey and cloudy, so there has been some reduction. it's not sludgy like a MM Nitro, but a little darker and more watery.
4x 25mL 40% NaOH have been added along the way, but that hsan't had much of an effect.
here are the reagent amounts used; the Aluminum is an 0.01mm/.004" thick oven liner chopped up to 1cm bits, and the ketone from a buffered performic and is suspected to be 75% (could do with a redistillation, i know) but it does yield when used in a MM Nitromethane AlHg. the MeAm.HCl is from chromic's unpublished procedure.
MDP2P 122g (suspected 91g ketone)
Al 36g
MeOH 600mL
HgCl2 230mg
dH20 169g
NaOH 53g
MeAm 90g
the NaOH and dH20 were mixed and allowed to cool. the MeAm.HCl was mixed in, and the NaCl was allowed to settle.
560mL MeOH was put in 3L 3N FB flask with 3" octagonal stir bar. the HgCl2 was added and disolved, then the Al was then added. after that started amalgamating for 45min, the MeAm/NaOH sol'n was added and allowed to mix. the ketone and 40mL of MeOH was put in an addition funnel and started a quick drip. after 25min the additon was complete and heat was added.
25mL of 40% NaOH solution was added at the 235m, 435m, 610m, and 720m marks.
the mixture will be left to stir overnight.
i learned a thing or two from charlie dontcha know.