HRID1025550

反应详情

EQUATION

反应方程式

HRID 1025550 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To the solution of 1-methyl-1H-imidazole (2 g, 24.4 mmol) in 16 mL of DCM was added dropwise 4.4 g of trichloroacetyl chloride and the resulting mixture was stirred at 25° C. for 6 h. The mixture was cooled to 0° C. and 3.4 mL of triethylamine was added dropwise with stirring. The solvent was evaporated and the residue was purified by flash column chromatography (petroleum ether/DCM=4/1) to give 2,2,2-trichloro-1-(1-methyl-1H-imidazol-2-yl)ethanone (3.1 g, yield 56%). 1H NMR (300 MHz, CDCl3) δ 7.35 (s, 1H), 7.16 (s, 1H), 4.06 (s, 3H).

WORKUP

后处理

  1. temperatureThe mixture was cooled to 0° C.
  2. stirringwith stirring
  3. customThe solvent was evaporated
  4. customthe residue was purified by flash column chromatography (petroleum ether/DCM=4/1)