HRID1414724

反应详情

EQUATION

反应方程式

HRID 1414724 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 20 parts of 2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one, 400 volume parts of acetic acid and 15 parts of 5% palladium-on-carbon is hydrogenated at atmospheric pressure and temperature under stirring. After 2600 volume parts of hydrogen is absorbed, the catalyst is removed by filtration. The filtrate is concentrated under reduced pressure and the residue is treated with diethyl ether to give 2,5,6,11-tetrahydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one as crystals. Recrystallization from ethanol gives colorless plates melting at 253° - 261° C.

WORKUP

后处理

  1. customAfter 2600 volume parts of hydrogen is absorbed
  2. customthe catalyst is removed by filtration
  3. concentrationThe filtrate is concentrated under reduced pressure
  4. additionthe residue is treated with diethyl ether