HRID1704196

反应详情

EQUATION

反应方程式

HRID 1704196 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

97.5 parts of p-tolylsulphonyl-acetonitrile are stirred together with 39 parts of sodium azide, 32 parts of ammonium chloride and 200 parts of dimethylformamide for 10 hours at 120°-130° C. The dimethylformamide is distilled off in vacuo, and the residue is dissolved in 1000 parts of water with the addition of sodium hydroxide to give pH 9. The solution is treated with animal charcoal, and precipitation is effected at pH 2-3 by the addition of hydrochloric acid. Recrystallisation of the precipitate from isopropanol yields 85 parts of 5-(p-tolylsulphonylmethyl)-tetrazole in the form of white crystals which melt at 206°-208°.

WORKUP

后处理

  1. distillationThe dimethylformamide is distilled off in vacuo
  2. dissolutionthe residue is dissolved in 1000 parts of water with the addition of sodium hydroxide
  3. customto give pH 9
  4. customRecrystallisation of the precipitate from isopropanol