反应详情

温度

140 °C

To a stirred suspension of 4-chloro-2,6-difluorobenzaldehyde (45 g, 255 mmol) in DMA (360 mL), at room temperature under nitrogen was added guanidine bis(carbonate) (70.0 g, 382 mmol). The mixture was heated to 140° C. for 3 hours. The reaction was then cooled to room temperature followed by addition of 400 mL water with stirring. The mixture was then filtered. The solids were then collected and triturated in 200 mL methanol for 10 minutes, then filtered. These solids were then dried in vacuo to obtain 31.6 g (63%) of 7-chloro-5-fluoroquinazolin-2-amine (82a) as a brown solid.

1. temperatureThe reaction was then cooled to room temperature
2. filtrationThe mixture was then filtered
3. customThe solids were then collected
4. customtriturated in 200 mL methanol for 10 minutes
5. filtrationfiltered
6. customThese solids were then dried in vacuo