HRID1422128

反应详情

EQUATION

反应方程式

HRID 1422128 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under a nitrogen atmosphere, 758 ml of pyridine and 469 g of dicalite were added to 6 l of dry dichloromethane. In one portion 469 g of chromium trioxide were added under vigorous stirring. The resulting mixture was stirred at room temperature for 0.5 h, after which a solution of 238 g of 2-(diethoxymethyl)-α-(2-fluorophenyl)-benzenemethanol in 600 ml dry dichloromethane was added. After stirring at room temperature for 2 h, the mixture was filtered. The filtrate was washed with 3×1 l of 1N sodium hydroxide in water and 1 l of water, dried over magnesium sulphate and evaporated to dryness under reduced pressure to yield 224 g of [2-(diethoxymethyl)phenyl](2-fluorophenyl)-methanone as an oil, M.S. (C.I.) (M/Z): 303 [M+H]+.

WORKUP

后处理

  1. stirringAfter stirring at room temperature for 2 h
  2. filtrationthe mixture was filtered
  3. washThe filtrate was washed with 3×1 l of 1N sodium hydroxide in water and 1 l of water
  4. dry with materialdried over magnesium sulphate
  5. customevaporated to dryness under reduced pressure