反应详情

A mixture of 5-amino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (1.5 g), 3-amino-3-methylpyrrolidine (0.76 g), DBU (0.77 g), and acetonitrile (30 ml) was refluxed for 7 hours. The precipitated crystals were collected by filtration after cooling, and washed with acetonitrile. The crystals were suspended in water (50 ml) and dissolved by addition of a 10% aqueous solution of acetic acid. The solution was treated with activated carbon, and adjusted to pH 7-8 with 10% aqueous ammonia. The precipitated crystals were collected by filtration, washed with water and then with ethanol, and dried to give 5-amino-7-(3-amino-3-methyl1-pyrrolidinyl)-1-cyclopropyl-6,8-difluoro-1,4-dihydro4-oxoquinoline-3-carboxylic acid (1.15 g), m.p. 271°-273° C. (decomp.).

1. temperaturewas refluxed for 7 hours
2. filtrationThe precipitated crystals were collected by filtration
3. temperatureafter cooling
4. washwashed with acetonitrile
5. dissolutiondissolved by addition of a 10% aqueous solution of acetic acid
6. additionThe solution was treated with activated carbon
7. filtrationThe precipitated crystals were collected by filtration
8. washwashed with water
9. dry with materialwith ethanol, and dried