HRID1655211

反应详情

EQUATION

反应方程式

HRID 1655211 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of m-chloroperbenzoic acid (1.61 g) in dichloromethane (75 ml) was added dropwise to a stirred solution of 2 -(4 -morpholino-3 -chloro-2 -pyridylmethylthio)-5 -methoxy- (1H)-benzimidazole (3.35 g) in dichloromethane (150 ml) cooled to -35°. After 1 hour, ammonia was passed through the solution for 5 minutes and the precipitate filtered off. The solution was evaporated under reduced pressure and the residue chromatographed (silica gel, 2 % CHCl3 /MEOH-NH3 ) to give an oil which was crystallised from ethanol to give 2 -(4 -morpholino-3 -chloro-2 -pyridylmethylsulphinyl)-5 -methoxy-(1H)-benzimidazole. (2.6 g).

WORKUP

后处理

  1. temperaturecooled to -35°
  2. filtrationthe precipitate filtered off
  3. customThe solution was evaporated under reduced pressure
  4. customthe residue chromatographed (silica gel, 2 % CHCl3 /MEOH-NH3 )
  5. customto give an oil which
  6. customwas crystallised from ethanol