Chemical Forums
Chemistry Forums for Students => Organic Chemistry Forum => Organic Chemistry Forum for Graduate Students and Professionals => Topic started by: rolnor on September 19, 2016, 08:10:37 AM
-
I Had use for HMPA when reacting isopropyl iodide with a enolate. I first tried DMPU but that did not work. Whe had an bottle of HMPA so I tried that and got a nice yield of alkylated material. I then wanted a safe substitute for HMPA and found in the literature that tripyrolidinephosphortriamide has similar properties. To make it dissolve 1 eq. of phosporoxytrichloride in diethyl ether under N2 and cool in icebath. Then add 6eq. of pyrolidine slowly, its exothermic. Then wait three hours and filter of the precipitated pyrolidine hydrochloride. Evaporate and distill the posphoramide at reduced pressure and its finnished. I have seen that you can buy this but its expensive. Maby this can be of use for somebody.
-
Whew, synthesizing your solvent, thats dedication.
-
It doesn't matter what P-N bond connections you have just that they are P-N bonds, and not P-O bonds. I would prefer to work with HMPA from a commercial source, then make my own solvent and have to purify it. Discard your gloves after use, wear a lab coat, keep the sash down, and wear a full face respirator if it makes you sleep easier.
-
It was faster to synthesize then order 8)