反应详情

温度

85 °C

A mixture of ethyl 1-((tert-butoxycarbonyl)(methyl)amino)-8-fluoro-6-iodo-4-oxo-1,4-dihydroquinoline-3-carboxylate (Preparation 35, 0.200 g), 37% aqueous formaldehyde (4.0 mL), and water (2.0 mL) is heated in an oil bath for 2.5 h at 85° C. The mixture is cooled, diluted with ice water (30 mL), and the resulting precipitate is collected, rinsed with ice water and partially air dried. The solid is dissolved in a mixture of acetone and CH2Cl2, dried (Na2SO4), and concentrated at reduced pressure to yield 0.194 g (90%) of the title compound as a white solid. Physical characteristics: MS (ESI+) m/z 421 (M+H)+; TLC (silica gel GF): Rf=0.32 acetone/CH2Cl2 (1/4).

1. temperatureThe mixture is cooled
2. customthe resulting precipitate is collected
3. washrinsed with ice water and partially air
4. customdried
5. dissolutionThe solid is dissolved in a mixture of acetone and CH2Cl2
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated at reduced pressure