HRID1712630

反应详情

EQUATION

反应方程式

HRID 1712630 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 0.170 g of 3-(1-trityl-1H-imidazol-4-yl)phenol, 4.5 ml of methanol, 1.5 ml of chloroform and 1.5 ml of 2N HCl is stirred at 55° C. for 2 hours. After cooling, the reaction mixture is admixed with 35 ml of aqueous saturated sodium hydrogencarbonate solution and extracted twice with 75 ml of dichloromethane. The combined organic phases are washed with 35 ml of brine, dried over sodium sulphate and concentrated by evaporation. The title compound is obtained as a white solid from the residue by means of flash chromatography (SiO2 60F). Rf=0.14 (200:10:1 dichloromethane-methanol-conc. ammonia); Rt=2.08.

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionextracted twice with 75 ml of dichloromethane
  3. washThe combined organic phases are washed with 35 ml of brine
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated by evaporation