HRID2179957

反应详情

EQUATION

反应方程式

HRID 2179957 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium hydride (141 mg, 60% dispersion in oil) was added to a solution of the product from step (b) (785 mg, 2.96 mmol) and 4-chloro-2,5-difluorobenzonitrile (546 mg, 3.75 mmol) in tetrahydrofuran (9 ml) and the resultant suspension was stirred for 0.5 h. The mixture was quenched with saturated aqueous ammonium chloride, basified to pH 8 and extracted with ethyl acetate (three times). The combined organic extracts were dried (sodium sulphate), evaporated and purified by chromatography on silica eluting with petrol—acetone to give 1.05 g (88%) of the sub-title compound as a colourless oil.

WORKUP

后处理

  1. customThe mixture was quenched with saturated aqueous ammonium chloride
  2. extractionextracted with ethyl acetate (three times)
  3. dry with materialThe combined organic extracts were dried (sodium sulphate)
  4. customevaporated
  5. custompurified by chromatography on silica eluting with petrol—acetone