HRID990815

反应详情

EQUATION

反应方程式

HRID 990815 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

640 mg of 1-benzyl-3-trimethylstannylindazole (1.72 mmol), 212 mg of 2-chloro-4,5-dimethylpyrimidine* (1.49 mmol) and 72 mg (0.10 mmol) of Pd(PPh3)2Cl2 (5.8 mol %) in 20 ml of toluene were heated under reflux overnight in an argon atmosphere. The mixture was cooled to room temperature, saturated ammonium chloride solution was added and the mixture was extracted with ethyl acetate. The organic phase was dried over magnesium sulphate and freed from the solvent on a rotary evaporator. Purification was carried out by chromatography over silica gel using cyclohexane/ethyl acetate as the eluent (gradient from 10:1 to 1:1).

WORKUP

后处理

  1. temperatureunder reflux overnight in an argon atmosphere
  2. extractionthe mixture was extracted with ethyl acetate
  3. dry with materialThe organic phase was dried over magnesium sulphate
  4. customfreed from the solvent on a rotary evaporator
  5. customPurification