HRID1957269

反应详情

EQUATION

反应方程式

HRID 1957269 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 3.5 g of 3-chloro-2-(4-chloro-3-chloroformylphenyl)-5-trifluoromethylpyridine in 10 ml of methylene chloride was added dropwise to 75 ml of a 40% by weight aqueous dimethylamine solution cooled to 0° C. The mixture was stirred at 0 to 5° C. for 4 hours and then diluted with 225 ml of water, after which it was extracted three times with 100 ml of tert-butyl methyl ether each time. The combined organic phases were washed twice with 100 ml of water each time, dried over sodium sulfate and concentrated. The residue was chromatographed on silica gel with cyclohexane/ethyl acetate (7:3). Yield: 2.2 g (61%) of colorless crystals; melting point: 90°-91° C.

WORKUP

后处理

  1. extractionafter which it was extracted three times with 100 ml of tert-butyl methyl ether each time
  2. washThe combined organic phases were washed twice with 100 ml of water each time
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. customThe residue was chromatographed on silica gel with cyclohexane/ethyl acetate (7:3)