反应详情

To the solution of sodium methoxide prepared from sodium (0.2 g) and absolute ethanol (9 ml) was added 1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl)-3-quinolinecarboxylic acid (0.5 g) and the mixture in sealed tube was heated for 72.5 hours at 140° to 150° C. After cooling, the reaction mixture was concentrated, water (4 ml) was added to the residue, and the solution was adjusted to pH 7 with acetic acid. The insoluble materials were filtered off and the filtrate was allowed to stand in a refrigeretor. The resulting precipitate was collected by filtration and recrystallized from dichloromethane-methanol (2:1; 6 ml) to give the title compound (0.12 g) as colorless prisms, mp 185°-187.5° C. (decompd.).

1. temperaturethe mixture in sealed tube was heated for 72.5 hours at 140° to 150° C
2. temperatureAfter cooling
3. concentrationthe reaction mixture was concentrated
4. additionwater (4 ml) was added to the residue
5. filtrationThe insoluble materials were filtered off
6. filtrationThe resulting precipitate was collected by filtration
7. customrecrystallized from dichloromethane-methanol (2:1; 6 ml)