HRID512934

反应详情

EQUATION

反应方程式

HRID 512934 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 5-[(3,5-Difluoro-phenyl)-hydroxy-methyl]-2-fluoro-benzonitrile (2.68 g, 10.2 mmol), 4-methylmorpholine N-oxide monohydrate (2.02 g, 15 mmol) and tetrapropylammonium perruthenate (35 mg, 0.1 mmol) in dry dichloromethane (50 mL) was stirred at room temperature for 2 hours. The reaction mixture was evaporated and the residue redissolved in ethyl acetate. The organic phase was washed with 10% sodium bisulphite and saturated ammonium chloride, dried and evaporated. Purification of the crude by chromatography over silica gel (EtOAc/hexane) afforded 2.05 g of the title compound (77% yield).

WORKUP

后处理

  1. customThe reaction mixture was evaporated
  2. dissolutionthe residue redissolved in ethyl acetate
  3. washThe organic phase was washed with 10% sodium bisulphite and saturated ammonium chloride
  4. customdried
  5. customevaporated
  6. customPurification of the crude by chromatography over silica gel (EtOAc/hexane)