HRID2059078

反应详情

EQUATION

反应方程式

HRID 2059078 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 13.7 parts by weight of 4,5-dichloroimidazole and 4.4 parts by weight of sodium hydroxide in 20 parts of water was added dropwise to a solution of 24.6 parts by weight of 2-chloro-N-chloromethyl-2',6'-dimethylacetanilide and 2.0 parts by weight of triethylbenzylammonium chloride in 50 parts by volume of dichloromethane at 20°-25° C., with vigorous stirring, which was continued for 2 hours. The organic phase was washed with three times 30 parts by volume of water, dried over sodium sulfate and evaporated under reduced pressure at 70° C., to give 29.9 parts by weight of 2-chloro-2',6'-dimethyl-N-(4,5-dichloroimidazol-1-yl-methyl)-acetanilide of melting point 99° C.; the product was pure according to the 1H-NMR spectrum and according to thin layer chromatography carried out with a 3:7 ethyl acetate:toluene mixture.

WORKUP

后处理

  1. washThe organic phase was washed with three times 30 parts by volume of water
  2. dry with materialdried over sodium sulfate
  3. customevaporated under reduced pressure at 70° C.