HRID26501
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was refluxed for 15 minutes
- filtrationThe Raney nickel was filtered off
- customthe solvent was removed from the filtrate
- additionTo the residue was added water