Quantitative determination of amine mixtures by multiplicative distribution. IX. Separation of organic bases by Craig distribution

Abstract

The sepn. of (+-)-BuNHCHPhCHPhNHBu, its meso isomer (I), iso-PrCHPhNHBu (II), PhCH2NHBu, and BuNH2, formed by reaction of benzylidenebutylamine with isopropylmagnesium halide in presence of MnCl2, by Craig after-fractionation processes in the solvent system CHCl3-MeOH-2% HCl (40:12:28) was complete after 95 steps in a distribution machine with 35 elements (E. Hecker, 1955). The over-all recovery was .apprx.93%; the deviation in the recovery of a single component was ?2%. The amines could be detd. even with incomplete sepn. after 54 steps by graphical evaluation of the overlapping distribution curves, if the portion of I was high enough (I > II). Temp. constancy was necessary.