反应详情

温度

80 °C

4-oxo-4H-3,1-benzoxazine-8-carboxylic acid derivative (51.5 g; 251.26 mmol) was dissolved in NH4OH (360.0 ml; 6.98 V; 28% solution). Ammonium acetate (77.5 g; 1.005 mmol) was added, and the reaction mixture was heated at 80° C. for 2 h. The reaction mixture was cooled to room temperature and diluted with MeOH (40 mL) then heated for 72 h at 80° C. in a pressure bottle. The reaction mixture was concentrated on the rotary evaporator then cooled on ice and filtered. The solid was dried under vacuum to provide the desired product (33.5 g, 65% yield).

1. temperatureThe reaction mixture was cooled to room temperature
2. temperaturethen heated for 72 h at 80° C. in a pressure bottle
3. concentrationThe reaction mixture was concentrated on the rotary evaporator
4. temperaturethen cooled on ice
5. filtrationfiltered
6. customThe solid was dried under vacuum