HRID1354391

反应详情

EQUATION

反应方程式

HRID 1354391 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product from step (a) (1.75 g) and 4-chloro-2,5-difluorobenzonitrile (1.86 g) in dry DMF (40 ml) were treated with 60% sodium hydride in mineral oil (470 mg) with stirring under nitrogen. The reaction mixture was stirred for 2.5 h, poured into water, and extracted with ethyl acetate. The extract was washed with water (5×) then brine and dried (MgSO4). The solvent was evaporated and the residue purified by chromatography (silica, 10% ether/isohexane as eluent) to give the sub-title compound (2.37 g) as a pale yellow oil.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred for 2.5 h
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with water (5×)
  4. dry with materialbrine and dried (MgSO4)
  5. customThe solvent was evaporated
  6. customthe residue purified by chromatography (silica, 10% ether/isohexane as eluent)