HRID1090402
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 suspension of 17.2 g (50 mmol) of 7-[(3oximino)cyclopentyl]-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 3.0 g of Raney-nickel and 300 ml of N,N-dimethylformamide was shaken in a hydrogen atmosphere at 45-50 psi for 24 hours. After removing the catalyst by filtration through Celite and addition of 100 ml of 6.0 M hydrochloric acid (60 mmol), the mixture was evaporated in high vacuo at 50°. The residue was triturated with a mixture of 200 ml of ethanol/ether (1:1) and the solid was removed by filtration, washed with ethanol/ether (1:1) and dried in vacuo to give 13.1 g of the title compound.
WORKUP
后处理
- customAfter removing the catalyst
- filtrationby filtration
- customthe mixture was evaporated in high vacuo at 50°
- customThe residue was triturated with a mixture of 200 ml of ethanol/ether (1:1)
- customthe solid was removed by filtration
- washwashed with ethanol/ether (1:1)
- customdried in vacuo