HRID461713
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationThe precipitated salt is filtered off
- customcrystallized from a mixture of ethanol and water (10 : 2 by volume)
- customyielding the crude salt form
- customThis fraction is recrystallized several times till constant rotation
- additionfrom a mixture of ethanol and water (10 : 2 by volume)