HRID1875773

反应详情

EQUATION

反应方程式

HRID 1875773 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-fluoro-4-hydroxy-benzonitrile (1.2 g, 8.7 mmol; CAS Reg. No. 405-04-9) in acetone (20 ml) was added cesium carbonate (4.2 g, 13.05 mmol) and 2-bromomethyl-benzoic acid methyl ester (2 g, 8.7 mmol; CAS Reg. No. 2417-73-4) and the resulting solution was heated to reflux for 12 h. The reaction mixture was filtered and evaporated in vacuo. The residue was purified by column chromatography over silica gel (8-10% ethyl acetate/n-hexane) to give the desired product as a yellow sticky solid (90%). MS (Turbo Spray): m/z=286.1 (M+H).

WORKUP

后处理

  1. temperature2417-73-4) and the resulting solution was heated
  2. temperatureto reflux for 12 h
  3. filtrationThe reaction mixture was filtered
  4. customevaporated in vacuo
  5. customThe residue was purified by column chromatography over silica gel (8-10% ethyl acetate/n-hexane)