FriendlyFinger - 1-6-2006 at 00:56
What's the right way to prepare 40% aqueous methylamine solution?
In Festers SOMM he says, mix 100g MeNH2.HCl in 50ml water chilled in a ice/salt to temp nearing 0 deg F. Then mix in cold 60g NaOH in 100ml water and
that's comparable to a comerical 40% solution.
Does that sound right to you?
Does Fester mean a 100mls of a 60% NaOH solution or 60g NaOH and 100ml of water?
0 deg F, that's -18 C. Does it have to be that cold!
[merged w/ MeAm thread by <u>same author</u> *wags finger* - Ramiel]
[Edited on 1-6-2006 by Ramiel]
MeNH2.HCl via EtOH. How man !!!
FriendlyFinger - 1-6-2006 at 01:28
I believe I have reached the point of total madness with this easy synth that I have attempted 19 times! using hexamine from different sources and
also making my own, as well as EtOH.
Then using alcohol from different sources, denatured, free from ketones, distilled vodka, my own brew etc. I also tried MeOH.
I have followed the proceedures posted on this site and never once have I had better than 50% yield, and never once have I distilled anywere near the
theoretical yield of ethyl formate.
And how about distill the formate at exactly 53 deg in 3 or 4 hours, as one person suggested No way! It always too me at least 9hrs to get less than
half and it took all my effort to keep it between 53 and 56 and that's with a Fenski packed column.
I just don't get it. How can anyone fail this easy synth 19 times. I even followed the patent as posted by Organikum using formalin and NH4Cl. I used
clean EtOH, I used clean real pure Hexamine, I used pure NH4Cl, good HCl. Am I the only one in the world that has failed 19 times!!!
[Edited on 1-6-2006 by FriendlyFinger]
bio2 - 1-6-2006 at 02:39
.... distill the formate at exactly 53 deg in 3 or 4 hours, as one person suggested No way! It always too me at least 9hrs to get less than half and
it took all my effort to keep it between 53 and 56.......
Obviously the person that said that had never done it!
It is as you say but up to 60deg or so is fine after the reflux.
Ethyl formate distills over at 54.5, water azeo 5% at 52.6 deg. As long as the 1-2 drops per second take-off is not exceeded you can go faster
although a 4.5L reaction took about 8 or 10 hours IIRC.
This doesn;t seem a failure as some also exagerate their yields although I would believe Org but not many others with 85%+ yields,
If it makes you feel any better, lol, Joe gets 70% or so after 3 many mole runs. That is recrystallized once from
EtOH using formaldehyde and all RA grade reagents.
FriendlyFinger - 2-6-2006 at 16:53
Well thanks for that and yes it does make me feel better, I'll get up off the floor and do it again.
Why were my 2 posts merged? did I do something wrong and why am I now a hazard, because I mentioned fester?
[Edited on 3-6-2006 by FriendlyFinger]