I have a "Hive Arc" but the searching is impossible. Does someone actually have it up and mirrored?
People way smarter than me write fancy books with big words and lame pictures so that we might advance the home production of methanamine. What is the netiquette approved naming here? IUPAC? Old School? Whatever? Wichever should have some common chemwords in the spellchecker.
I can tell you I would rather deal with potentially explosive complexes all day then spend 10 minutes with formaldehyde filling a room, not that I have ever done that, twice.
From my brief experience with iron and nitromethane, I say there are only a few points to push this to number one on the list if you can get/distill nitromethane, and I think that is everyone.
First, starter broth of iron, iron chloride, water and some small amount of HCl, much less than Elusis' starting amount, in a flask setup for reflux with mechanical stirring.
Second, the addition of nitromethane to this mix, along with HCl to keep it slightly acidic, the methylamine a salt and the iron rocking, but in a controlled manner, dripping probably, but possibly dripping the nitro and HCl out of different funnels. Needing 4 or 5 necks or a menorah setup triple with claisens but do-able.
Third, fresh additions of iron.
So, the amount of HCl added with the nitro is mol easy or could be monitored by pH. Can nitromethane hang out in a funnel for a while with conc. HCl without something bad happening? I would err on the side of caution and add it separately unless someone here could show me different.
Sure nitromethane reactions can be vigorous, but that helps push to completion. Elusis "Reflux for 12hrs" or whatever nonsense goes counter to all thought. Looking at other reductions of nitro groups with iron, iron chloride and acid or no, that 12hrs is insane. Looks can be deceiving, but nitromethane reacts volcano style fast if you throw in too much with fine iron powder. Not that I have ever done that stupid move. Or thrown DCM into hot freshly basified stuff. Or thrown away 10,000 mag stirrers with filtered trash on accident then had to dig through hazmat because I wasn't going to have to say I threw another magstirrer away, again. Or superheated a mix then hit warp speed on the mag stirrer.
Right, so nitro groups reduce quickly, at least most of the way, as my reading goes. I bet Hudlickey or OrgSyn could be followed close, with the mods I wrote about.
If I get to it I will post results or proof of my stupidity, whatever.
Anyone with pointers, please speak up. Or if you have that bit of Hive Gold and would like to share the details, I'm sure I'm not the only person who would like to read it. I would also like to read the fabled hive works of vacuum refluxing formaldehyde/ammCl. 90% Rhodium? Says who? In 4 hours? Whatever, if it is happening, my test says it is happening slow. In fairness, I did not have the same amount of pressure.
In case you didn't read this the first time and are as stupid as me, DO NOT POUR NITROMETHANE INTO REFLUXING IRON/IRON CHLORIDE/HYDROCHLORIC ACID! Drip... Slowly... Then judge. Not even a "I'm just going to pour in a little to see if this takes off" because it will. It is really sad watching the way a beautiful Ahlinn fills with stuff. You even have a few seconds to ponder how many CFM your vent fan is, what explosion proof motor means, when your fire extinguisher was last charged and whether ABC covers all of the bad shit nitromethane acid vapor is about to throw at you. It actually turned out to be a non-issue, mostly because my gear is pro, even if I am not always. I live to make different exciting new mistakes!
While I was writing this Douchermann posted and I can tell you from experience that nitro reacts with this mix. Perhaps an alcohol might speed things along and get everyone sexy. It helps me mingle. One thing I was wondering about was whether intermediates in the reduction might be less or more soluble, but I would guess more sol because the c# and polar -OH. But I don't know.