HRID2268585

反应详情

EQUATION

反应方程式

HRID 2268585 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 3-chloro-N-(3,5-difluoro-phenyl)-5-methoxy-N-propyl-benzamide (0.164 g) in anhydrous dichloromethane (5 ml) at −78° C. was added 1M boron tribromide solution in dichloromethane (3.5 ml). The reaction mixture was stirred at this temperature for 15 min. The reaction was allowed to warm to room temperature, and after 3.5 h the reaction was cooled to −78° C. and methanol (6 ml) added. The reaction was allowed to rewarm to room temperature and the solvent removed in vacuo. The residue was purified by flash column chromatography eluting with cyclohexane:ethyl acetate (3:1 v/v) to give the title compound as a colourless oil (0.110 g).

WORKUP

后处理

  1. temperatureafter 3.5 h the reaction was cooled to −78° C.
  2. customto rewarm to room temperature
  3. customthe solvent removed in vacuo
  4. customThe residue was purified by flash column chromatography
  5. washeluting with cyclohexane:ethyl acetate (3:1 v/v)