HRID1651595

反应详情

EQUATION

反应方程式

HRID 1651595 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 17.2 g (50 mmol) of 7-[(3-oximino)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

  1. customAfter removing the catalyst
  2. filtrationby filtration
  3. customthe mixture was evaporated in high vacuo at 50°
  4. customThe residue was triturated with a mixture of 200 ml of ethanol/ether (1:1)
  5. customthe solid was removed by filtration
  6. washwashed with ethanol/ether (1:1)
  7. customdried in vacuo