HRID1370517

反应详情

EQUATION

反应方程式

HRID 1370517 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
145 °C

PROCEDURE

实验过程

To solution of 2,4-dichlorobenzothiazole (255, 2.23 g, 11 mmol) and 4-amino-2,6-dichlorophenol (Aldrich, 1.78 g, 10 mmol) in 10 mL of DMSO was add K2CO3 (Aldrich, 4.14 g, 30 mmol). The mixture was heated at 145° C. for 4 h. After cooled to room temperature, the reaction mixture was diluted with EtOAc (300 mL) and filtered through a pad of silica gel and activated carbon followed by washing with EtOAc (500 mL). The filtrate was concentrated and the residue was purified by chromatography (20%-30% EtOAc/Hexanes) to give 1.15 g (33%) of product.

WORKUP

后处理

  1. temperatureAfter cooled to room temperature
  2. filtrationfiltered through a pad of silica gel and activated carbon
  3. washby washing with EtOAc (500 mL)
  4. concentrationThe filtrate was concentrated
  5. customthe residue was purified by chromatography (20%-30% EtOAc/Hexanes)