反应详情

To a solution of sodium methoxide prepared from sodium (0.4 g) and absolute methanol (20 ml) was added 1-cyclopropyl-6,8-difluoro-1,4-dihydro-7-(3-methyl-1-piperazinyl)-4-oxo-3-quinolinecarboxylic acid (1.12 g), and, the mixture in sealed tube was stirred for 70.5 hours at 140° to 150° C. and then concentrated. The residue was dissolved in small amount of water, the resulting solution was adjusted to pH 7 with acetic acid and concentrated. The resulting residue was purified by silica gel column chromatography eluting with chloroform-methanol-concentrated aqueous ammonia (20:6:1) and recrystallized from methanol to give the title compound (0.33 g) as pale yellow prisms, mp 162°- C.

1. concentrationconcentrated
2. dissolutionThe residue was dissolved in small amount of water
3. concentrationconcentrated
4. customThe resulting residue was purified by silica gel column chromatography
5. washeluting with chloroform-methanol-concentrated aqueous ammonia (20:6:1)
6. customrecrystallized from methanol