反应详情

A mixture of 480 mg of 7-chloro-1-ethyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid, 1.0 g of 2-dimethylaminomethylpiperazine and 5 ml of pyridine in a sealed flask flushed with argon was stirred at 120°-130° C. for 18 hours. The solvent was removed in vacuo. The residue was evaporated twice from toluene, giving a gum. The gum was added to a silica gel column and flash chromatographed with methanol:chloroform (1.5:8.5 saturated with water). Fractions 61 and 62 were combined, evaporated and dried, giving 105 mg of the desired product as a white solid, mp 148°-150° C.

1. customflushed with argon
2. customThe solvent was removed in vacuo
3. customThe residue was evaporated twice from toluene
4. customgiving a gum
5. additionThe gum was added to a silica gel column and flash
6. customchromatographed with methanol:chloroform (1.5:8.5 saturated with water)
7. customevaporated
8. customdried