反应详情

温度

40 °C

Under nitrogen atmosphere, a solution of 2-fluoro-3-hydroxy-5-methoxybenzaldehyde (17.01 g, 100 mmol), 4-aminobenzonitrile (11.81 g, 100 mmol), and guanidine hydrochloride (287 mg, 3 mmol) in methanol (85 mL) was stirred at 40° C. for 1.5 hours. Trimethylsilylcyanide (18.1 mL, 130 mmol) was then added dropwise thereto, and the resulting mixture was stirred at 40° C. for 22 hours. After cooling the mixture, under cooling at 15° C., 3% aqueous sodium hydrogen carbonate solution (87.65 g) was added dropwise thereto, and the resulting mixture was stirred for 1 hour under cooling at 10° C. The precipitated solid was filtered and dried to obtain the captioned compound (27.91 g) as a white solid.

1. temperatureAfter cooling the mixture
2. temperatureunder cooling at 15° C.
3. stirringthe resulting mixture was stirred for 1 hour
4. temperatureunder cooling at 10° C
5. filtrationThe precipitated solid was filtered
6. customdried