HRID1414724
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
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
- customAfter 2600 volume parts of hydrogen is absorbed
- customthe catalyst is removed by filtration
- concentrationThe filtrate is concentrated under reduced pressure
- additionthe residue is treated with diethyl ether