HRID28095

反应详情

EQUATION

反应方程式

HRID 28095 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The cyanohydrin of 4-fluoro-3-phenoxybenzaldehyde (0.038 mol) is dissolved in 150 ml ether and cooled to 0° in an ice bath. To this is slowly added methanesulfonyl chloride in 20 ml ether. The mixture is stirred for 10 minutes then triethylamine in 20 ml ether is added dropwise. The solution turns white, and a precipitate appears. The reaction mixture is kept at 0° over-night and is then worked up with water and extracted with ether. The ether phase is washed with 30% sodium bisulfite solution (2×), ether and water (2×), and dried over sodium sulfate. The mixture is filtered and the filtrate concentrated to give α-cyano-4 fluoro-3-phenoxybenzyl methanesulfonate.

WORKUP

后处理

  1. temperaturecooled to 0° in an ice bath
  2. waitThe reaction mixture is kept at 0° over-night
  3. extractionextracted with ether
  4. washThe ether phase is washed with 30% sodium bisulfite solution (2×), ether and water (2×)
  5. dry with materialdried over sodium sulfate
  6. filtrationThe mixture is filtered
  7. concentrationthe filtrate concentrated