HRID1736771

反应详情

EQUATION

反应方程式

HRID 1736771 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2 g (3 mmol) of 4'-[(2-n-butyl-benzimidazol-1-yl)-methyl]-2-(1-triphenylmethyl-tetrazol-5-yl)-biphenyl are dissolved in a mixture of 10 ml of methylene chloride and 10 ml of methanol, treated with 10 ml of etherified hydrochloric acid and stirred at ambient temperature for 3 hours. The mixture is rotary evaporated to dryness in vacuum. The residue is dissolved in methanol, rendered alkaline using ammonia and rotary evaporated once again. The crude product is purified over a silica gel column (grain size: 0.063-0.2 mm, eluting agent: methylene chloride/ethanol/ammonia=19:1:0.1). The product is crystallised from ether and dried at 50° C. in vacuum.

WORKUP

后处理

  1. customThe mixture is rotary evaporated to dryness in vacuum
  2. dissolutionThe residue is dissolved in methanol
  3. customrotary evaporated once again
  4. customThe crude product is purified over a silica gel column (grain size: 0.063-0.2 mm, eluting agent: methylene chloride/ethanol/ammonia=19:1:0.1)
  5. customThe product is crystallised from ether
  6. customdried at 50° C. in vacuum