HRID1162929

反应详情

EQUATION

反应方程式

HRID 1162929 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triphenylphosphine (940 mg, 3.59 mmol) and carbon tetrabromide (1.19 g, 3.59 mmol) were added to a methylene chloride solution (10 ml) that contained the 7-(3-hydroxypropylamino)-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one (500 mg, 1.38 mmol) obtained in step B of Example 1-49. The obtained mixture was stirred at a room temperature for 3 hours. The reaction solvent was distilled away, and the obtained residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:2 to 1:1), so as to obtain 7-(3-bromopropylamino)-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one (245 mg, 42%).

WORKUP

后处理

  1. distillationThe reaction solvent was distilled away
  2. customthe obtained residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:2 to 1:1)