HRID1111161

反应详情

EQUATION

反应方程式

HRID 1111161 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution containing alpha-bromo-4-tolunitrile (19.6 g) and 1,2,4-triazole (30.5 g) in a mixture of chloroform (250 mL) and acetonitrile (50 mL) is stirred at reflux for 15 hours. The solution is cooled and washed with 3% aqueous sodium bicarbonate (200 mL) and the organic solution is then dried (MgSO4) and evaporated. The residue is chromatographed on silica gel (300 g). Elution with chloroform/isopropanol (10:1) affords 4-[1-(1,2,4-triazolyl)methyl]-benzontrile, m.p. 77°-79°, which forms a hydrochloride salt, m.p. 200°-205°, when its solution in ethyl acetate is treated with ethereal HCl.

WORKUP

后处理

  1. temperatureat reflux for 15 hours
  2. temperatureThe solution is cooled
  3. washwashed with 3% aqueous sodium bicarbonate (200 mL)
  4. dry with materialthe organic solution is then dried (MgSO4)
  5. customevaporated
  6. customThe residue is chromatographed on silica gel (300 g)
  7. washElution with chloroform/isopropanol (10:1)