HRID1059144

反应详情

EQUATION

反应方程式

HRID 1059144 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

1-(4′-Chloro[1,1′-biphenyl]-3-yl)-2-methyl-1-(1-trityl-1H-imidazol-4-yl)-1-propanol (0.71 g) and pyridine hydrochloride (0.25 g) were dissolved in methanol (20 ml), and the mixture was stirred at 60° C. for 2 h. To the reaction mixture was added saturated aqueous sodium hydrogen carbonate solution and the mixture was concentrated. Water and ethyl acetate were added and the mixture was extracted with ethyl acetate. The organic layer was dried and concentrated, and the obtained residue was purified by silica gel column chomatography (eluent, dichloromethane:methanol=40:1). Recrystallization from hexane-ethyl acetate gave the title compound (0.31 g) as a colorless solid.

WORKUP

后处理

  1. concentrationthe mixture was concentrated
  2. additionWater and ethyl acetate were added
  3. extractionthe mixture was extracted with ethyl acetate
  4. customThe organic layer was dried
  5. concentrationconcentrated
  6. customthe obtained residue was purified by silica gel column chomatography (eluent, dichloromethane:methanol=40:1)
  7. customRecrystallization from hexane-ethyl acetate