tag:blogger.com,1999:blog-4387100009341358284.post917868498031958747..comments2024-03-12T09:55:15.923+01:00Comments on Curly Arrow: How to make a primary amide - The Ley WayDaniel Sejerhttp://www.blogger.com/profile/12498255536497699232noreply@blogger.comBlogger5125tag:blogger.com,1999:blog-4387100009341358284.post-25856533469840317362009-03-20T01:00:00.000+01:002009-03-20T01:00:00.000+01:00This reaction actually has a significant exotherm ...This reaction actually has a significant exotherm early on and can be extemely dangerous to run an any type of scale if you don't control this first exotherm associated with the formation of NH3. I recently was a witness to the damage a 800mg scale reaction can make. I would never run this reaction on anything bigger than 50mg.Anonymousnoreply@blogger.comtag:blogger.com,1999:blog-4387100009341358284.post-88187067897059901462008-08-20T21:59:00.000+02:002008-08-20T21:59:00.000+02:00There is another method for mild aminolysis that u...There is another method for mild aminolysis that uses NH4Cl + Me3Al 1:1 in anhydrous conditions and RT to 40C and Ar. I think the method comes from Weinreb. It works very nicely with primary and secondary aliphaic amines too (preferably used as free base, not a hydrochloride)<BR/><BR/>Mg-nitride is a better workup of course and the reagent got to be cheap, it is made readily from the elements - milkshakehttps://www.blogger.com/profile/08188961610554710616noreply@blogger.comtag:blogger.com,1999:blog-4387100009341358284.post-2973887433893702112008-08-20T21:05:00.000+02:002008-08-20T21:05:00.000+02:00Nice method. I tried to make amides from ethyl est...Nice method. I tried to make amides from ethyl esters using 7N ammonia in methanol in a sealed tube. Works fine but sometimes takes longer time to complete.Anonymousnoreply@blogger.comtag:blogger.com,1999:blog-4387100009341358284.post-56303286452721748312008-08-20T09:25:00.000+02:002008-08-20T09:25:00.000+02:00Hmmmm yes. I think I prefer the method that doesn'...Hmmmm yes. I think I prefer the method that doesn't involve bombs. D!Daniel Sejerhttps://www.blogger.com/profile/12498255536497699232noreply@blogger.comtag:blogger.com,1999:blog-4387100009341358284.post-89843300127631735982008-08-20T03:07:00.000+02:002008-08-20T03:07:00.000+02:00It's an annoying exercise making the solution and ...<EM>It's an annoying exercise making the solution and the actual reaction CO2R to CONH2 doesn't really work that well.</EM><BR/><BR/>This is why we have Parr Bombs. If a sealed tube does not work, then 200 C and 600 psi most likely will.Milohttps://www.blogger.com/profile/06753588919496192713noreply@blogger.com