HRID1388914

反应详情

EQUATION

反应方程式

HRID 1388914 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.65 grams of α-methyl-1H-benzimidazole-1-propanamine and 1.82 grams of 1-[4-(2-amino-2-oxoethyl)phenoxy]-2,3-epoxypropane in 6 ml. of 95 percent methanol was refluxed for 19 hours. The solvent was evaporated from the mixture and the residual solid was triturated several times with ether. The solid was then dried and chromatographed on a silica gel column using methanol. The fractions containing the desired product were determined by thin-layer chromatography and combined. The solvent was then evaporated to leave a residual oil which solidified on cooling to give N-{3-[4-(2-amino-2-oxoethyl)phenoxy]-2-hydroxypropyl}-α-methyl-1H-benzimidazole-1-propanamine melting at about 139°-142° C. This compound has the following structural formula. ##STR18##

WORKUP

后处理

  1. customThe solvent was evaporated from the mixture
  2. customthe residual solid was triturated several times with ether
  3. customThe solid was then dried
  4. customchromatographed on a silica gel column
  5. additionThe fractions containing the desired product
  6. customThe solvent was then evaporated
  7. customto leave a residual oil which
  8. temperatureon cooling