Well K.C., it's like this. His main trip is that he really really likes the concept of cutting out one whole procedure by combining it with another. It appeals to his sense of efficiency, or something. Also, because it is the first and only reduction he has ever attempted, he feels a certain drive to master it. He would like to feel he has it pretty well down before moving on. Call it a work ethic if you want.
He also tried making MeNH2 via the Sumerian vac reflux thing and failed, and I guess he feels a little intimidated and frustrated by it (at least that reaction), making the in-situ deal look that much better. I know it's not logical, but what can I say.
I suppose he'd be willing to try the other methylamine synth that's supposed to be pretty easy, which one is it, the formaldehyde and ammonium chloride one? And I'm sure he'll find it to be a breeze, but damn, he just would like to get this nitro/Al/Hg thing down if possible.
So a mild 50C reflux eh? Shit, not possible with Reynolds Hotbags---that reaction just goes too nuts and the aluminum is 90% broken down within 40 minutes or so. And that's even with the aluminum ground into little nuggets; if it was left as open squares it would be way too crazy. At the peak moment, the refluxing MeOH is *pouring* down from the condenser!
It has become obvious that he needs to use some thicker aluminum than foil, but still doesn't have enough info to visualize what's going to happen with it. Can you give an overview of roughly what one should expect in the way of the timing when using pie plates? This would help a lot. For example: with pie-plate thickness aluminum, will it
A) never bubble at all
B) only bubble slightly
C) only bubble slightly, but after 3 hours
C) end up bubbling hard, but after 3 hours
etc. etc. Know what I mean? I need to know what's going to happen so that he doesn't think it's not working and cancel it or something. And no one really states these physical/timing details. My concern is that since I've read that the critical part of the reaction is over when the bubbling stops. SO I assume that one would to have all their ketone in by that time.
Am I making any sense?? I really need to understand the timing of this (with thicker Al)!