Quote: Originally posted by chemist1243 | Quote: Originally posted by PirateDocBrown | Why do you not do an extraction with an immiscable organic solvent? (Make some 1,4 dioxane, or distill some starter fluid for ether. Never handle
amines in halogenated solvents.)
Why do you let it stand for 2 days (!) before reflux? Surely reflux would provide much faster reaction as well as the ability for the reactants to
comingle.
[Edited on 11/25/19 by PirateDocBrown] |
i guess diethyl ether could work, but unfortunately, my colum is broke atm. i was planning to recover some diethyl ether from starting fluid soon, but
i guess thats gonna have to wait for a new colum.
as for me waiting 2 days? its been a very wet and cold november where i live. i dont have a fumehood, so i have to go outside for most distillations,
which at this time of the year is rare due to such poor weather conditions.
a 55*C reflux for like 5 hours shouldve done it, but ill take what i can get. thats mostly why i refluxed the daylight out of it as soon as i could
for as long as i could |
You don't need a fume hood to do distillations, unless you're working with something particularly noxious or otherwise hazardous to health. Place some
tubing on the vacuum take off adapter and lead it out of a nearby window. I've done hundreds of distillations like this with all sorts of organic
solvents, and even azeotropic HCl.
[Edited on 11-25-2019 by monolithic] |