HRID1398889

反应详情

EQUATION

反应方程式

HRID 1398889 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 methyl 3-amino-2-[(4-hydroxybutyl)amino]benzoate (29.8 g, 125 mmol) in dichloromethane (500 mL) was added N-chlorosuccinimide (33.3 g, 250 mmol) at room temperature. After 4 h, the reaction mixture was quenched with aqueous sodium hydrogen carbonate and purified by flash column chromatography on silica gel eluting with a 30% ethyl acetate/n-hexane mixture to give the title compound as a pale red solid (5.81 g, 21.3 mmol, 17%).

WORKUP

后处理

  1. customthe reaction mixture was quenched with aqueous sodium hydrogen carbonate
  2. custompurified by flash column chromatography on silica gel eluting with a 30% ethyl acetate/n-hexane mixture