HRID50116

反应详情

EQUATION

反应方程式

HRID 50116 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

In a 500 ml flask a mixture of 200 ml of dry ethanol, 20 g (0.026 mol) of 2-n-butyl-4-chloro-1-[(2′-(2-triphenylmethyl -2H-tetrazol-5-yl)-1,1′-biphenyl-4-yl)-methyl]1H-imidazol-5-methanol methyl-isobutyl ketone solvate and 1.45 g (0.026 mol) of potassium hydroxide was refluxed for 9 h, treated with 0.5 g of charcoal and filtered. The filtrate was concentrated to a volume of 30 ml under diminished pressure, and after addition of 150 ml of acetonitrile again to a volume: of 60 ml. The suspension was stirred at 0° C. for 1 h, the precipitated crystals were filtered, washed twice with 25 ml of cold acetonitrile and dried at 70° C. to give 10.6 g (88%) of the title compound.

WORKUP

后处理

  1. temperaturewas refluxed for 9 h
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated to a volume of 30 ml under diminished pressure
  4. additionafter addition of 150 ml of acetonitrile again to a volume
  5. filtrationthe precipitated crystals were filtered
  6. washwashed twice with 25 ml of cold acetonitrile
  7. customdried at 70° C.