反应详情

0.75 g (2.7 mmole) of 9,10-difluoro-2,3-dihydro3-methyl-7-oxo-7H-pyrido[1,2,3-de]-1,4-benzoxazine-6-carboxylic acid, 40 ml acetonitrile and 1.03 g (8.00 mmole) of N-ethyl-3-pyrrolidinemethanamine were refluxed overnight. The reaction mixture was cooled in an ice bath and then filtered. The precipitate was washed with ethanol/ether (4:1), and then with ether until dry to give 0.86 g of 10-[3-[(ethylamino)methyl]-1-pyrrolidinyl]-9-fluoro-2,3-dihydro-3-ethyl-7-oxo-7H-pyrido[1,2,3-de]-1,4-benzoxazine-6-carboxylic acid, mp 221°-224° C. Analysis for C20H21FN3O4.1/2H2O C, 60.29; H, 6.33, N, 10.55 Found C, 60.45, H, 6.21, N, 10.80

1. temperatureThe reaction mixture was cooled in an ice bath
2. filtrationfiltered
3. washThe precipitate was washed with ethanol/ether (4:1)
4. dry with materialwith ether until dry