HRID461713

反应详情

EQUATION

反应方程式

HRID 461713 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of 20 parts of p-(2-thenoyl)hydratropic acid and 9.3 parts of (-)-α-methylbenzylamine in 200 parts of ethanol are added 50 parts of water. The precipitated salt is filtered off and crystallized from a mixture of ethanol and water (10 : 2 by volume), yielding the crude salt form. This fraction is recrystallized several times till constant rotation, from a mixture of ethanol and water (10 : 2 by volume), to yield (-)-p-(2-thenoyl)hydratropic acid α-methylbenzylamine; m.p. 170.5° C.; [α](1.98% MeOH) = -13.74°.

WORKUP

后处理

  1. filtrationThe precipitated salt is filtered off
  2. customcrystallized from a mixture of ethanol and water (10 : 2 by volume)
  3. customyielding the crude salt form
  4. customThis fraction is recrystallized several times till constant rotation
  5. additionfrom a mixture of ethanol and water (10 : 2 by volume)