HRID1902455

反应详情

EQUATION

反应方程式

HRID 1902455 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4.16 grams of 2-methyl-1H-benzimidazole-1-propanamine and 4.56 grams of 1-[4-(2-amino-2-oxoethyl)phenoxy]-2,3-epoxypropane in 50 ml of 90% methanol was refluxed for 22 hours. The solvent was then evaporated to leave a thick oil which was 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 evaporated to leave a thick oily residue which solidified partially on standing. This was recrystallized from ethanol to give N-{3-[4-(2-amino-2-oxoethyl)phenoxy]-2-hydroxypropyl}-2-methyl-1H-benzimidazole-1-propanamine melting at about 146°-149° C. This compound has the following structural formula: ##STR14##

WORKUP

后处理

  1. temperaturewas refluxed for 22 hours
  2. customThe solvent was then evaporated
  3. customto leave a thick oil which
  4. customwas chromatographed on a silica gel column
  5. additionThe fractions containing the desired product
  6. customThe solvent was evaporated
  7. customto leave a thick oily residue which
  8. customThis was recrystallized from ethanol