HRID730177

反应详情

EQUATION

反应方程式

HRID 730177 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
115 °C

PROCEDURE

实验过程

A stirred mixture of 5-bromo-2-[2-(3-methoxy-2-methyl-phenyl)-ethyl]-phenylacetonitrile 10 (8.57 g; 24.9 mmol) in water and acetic acid was treated drop-wise with concentrated sulfuric acid (8.5 mL), heated at 115° C. for 5 hours, cooled to ambient temperature, diluted with water and extracted with chloroform. The extracts were combined, dried over Na2SO4, and evaporated. The resultant residue was purified on a silica gel column (hexane and ethyl acetate (7:3) as eluent) to give compound 11, 5.0 g, 55% yield.

WORKUP

后处理

  1. temperaturecooled to ambient temperature
  2. extractionextracted with chloroform
  3. dry with materialdried over Na2SO4
  4. customevaporated
  5. customThe resultant residue was purified on a silica gel column (hexane and ethyl acetate (7:3) as eluent)