反应详情

To a solution of sodium methoxide prepare from sodium (0.2 g) and absolute methanol (10 ml) was added 7-(3-amino-1-pyrrolidinyl)-1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxo-3quinolinecarboxylic acid (0.47 g) and the mixture in sealed tube was stirred for 49 hours at 140° to 150° C. and then concentrated. The residue was purified by silica gel column chromatography eluting with chloroform-methanol-concentrated aqueous ammonia (20:6:1) and recrystallized from a solution of dichloromethanemethanol (1:1) to give the title compound (6 mg) as pale yellow prisms, mp 207.5°-212° C.

1. concentrationconcentrated
2. customThe residue was purified by silica gel column chromatography
3. washeluting with chloroform-methanol-concentrated aqueous ammonia (20:6:1)
4. customrecrystallized from a solution of dichloromethanemethanol (1:1)