HRID17148
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A solution of Example 277B (10,25 g, 42.1 mmol) in POCl3 (50 mL) was stirred at reflux for 2 hours, cooled to room temperature, diluted with ice water, and stirred vigorously resulting in a precipitate which was collected by filtration. The filter cake was further purified by silica gel chromatography on silica gel with dichloromethane to provide 7.14 g (64% yield) of the desired product. MS (ESI(+)) m/e 261.9, 263.9 (M+H)+.
WORKUP
后处理
- temperatureat reflux for 2 hours
- customresulting in a precipitate which
- filtrationwas collected by filtration
- customThe filter cake was further purified by silica gel chromatography on silica gel with dichloromethane