HRID26501

反应详情

EQUATION

反应方程式

HRID 26501 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 1.15 g of 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine in 20 ml of ethanol was added 6 ml of Raney nickel (wet) and the mixture was refluxed for 15 minutes under stirring. The Raney nickel was filtered off and the solvent was removed from the filtrate. To the residue was added water. By this procedure was obtained 11H-s-triazolo[3,4-b][3]benzazepine as crystals. Recrystallization from ethanol-n-hexane yielded colorless needles, m.p. 157°-158° C. The infrared absorption spectrum was identical with the spectrum of the same compound obtained by reacting 2-hydrazino-3-benzazepine with ortho-formic acid ester.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 15 minutes
  2. filtrationThe Raney nickel was filtered off
  3. customthe solvent was removed from the filtrate
  4. additionTo the residue was added water