HRID619680

反应详情

EQUATION

反应方程式

HRID 619680 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 12.3 g of 1-(4-chlorophenyl)-2-pyridin-4-yl-ethanedione and 7.4 g of 2,4,6-trimethylbenzaldehyde in 125 ml of acetic acid containing 40 g of ammonium acetate was stirred at 100° C. for 2 hours, then left to cool to room temperature. The mixture was poured into a mixture of 300 ml of ice-water and 200 ml of concentrated ammonia solution and the mixture was extracted three times with ethyl acetate. After drying over anhydrous magnesium sulphate the solvent was evaporated. The residue was purified by chromatography on silica gel with dichloromethane/methanol (9:1) and crystallized from ethyl acetate to yield 6.7 g of 4-[5-(4-chlorophenyl)-2-(2,4,6-trimethyphenyl)imidazol-4-yl]pyridine, m.p. 275° C.

WORKUP

后处理

  1. waitleft
  2. temperatureto cool to room temperature
  3. extractionthe mixture was extracted three times with ethyl acetate
  4. dry with materialAfter drying over anhydrous magnesium sulphate the solvent
  5. customwas evaporated
  6. customThe residue was purified by chromatography on silica gel with dichloromethane/methanol (9:1)
  7. customcrystallized from ethyl acetate