HRID2198782

反应详情

EQUATION

反应方程式

HRID 2198782 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Chloro-4-(4-chlorophenyl)-2-butanone (110 g) was added portionwise over half an hour to a stirred suspension of imidazole (175 g) in dimethylformamide (150 ml) at 0° C. and the mixture stirred overnight at ambient temperature. The resulting solution was poured into wate (1500 ml) with seeding at the first sign of turbidity, and the precipitate filtered off and washed well with water and hexane. Chromatography of the product on silica gel (1 Kg), eluting with 7% methanol in methylene chloride gave 100 g of 1-[4-(4-chlorophenyl) butan-2-on-1-yl]imidazole. The hydrochloride salt from acetone/methanol had a m.p. of 172.5°-174° C.

WORKUP

后处理

  1. additionThe resulting solution was poured into wate (1500 ml)
  2. filtrationthe precipitate filtered off
  3. washwashed well with water and hexane
  4. washChromatography of the product on silica gel (1 Kg), eluting with 7% methanol in methylene chloride