HRID552580

反应详情

EQUATION

反应方程式

HRID 552580 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-Bromo-3-methanesulfonyl-benzene (11.0 mmol) (see Intermediate 11) and 4-hydroxy-benzoic acid methyl ester (1.2 mmol) are dissolved in toluene (0.1M). Palladium acetate (0.02 mmol), biphenyl-2-yl-di-tert-butyl-phosphane (0.03 mmol) and tri-basic potassium phosphate (2.0 mmol) are added and the reaction heated reaction at 90° C. for 18 h. The reaction is allowed to cool to room temperature, washed with water while and then the aqueous extracted with dichloromethane. The organic portions are combined and concentrated in vacuo and purified by radial silica chromatography, eluting with ethyl acetate and hexane.

WORKUP

后处理

  1. temperaturethe reaction heated
  2. customreaction at 90° C. for 18 h
  3. washwashed with water while and then the
  4. extractionaqueous extracted with dichloromethane
  5. concentrationconcentrated in vacuo
  6. custompurified by radial silica chromatography
  7. washeluting with ethyl acetate and hexane