反应详情

温度

100 °C

To a stirred solution of polyphosphoric acid (20 g) at 100° C. was added N-(2-fluoro-5-methoxyphenyl)urea (900 mg, 4.89 mmol) over 5 minutes followed by cyclohexanone (719 mg, 7.33 mmol) in one portion under N2. The mixture was stirred at 100° C. for 2 hours, cooled to 35° C. and quenched into water (400 mL). The crude product was filtered and washed with water (100 mL). The isolated solid was slurred in a mixture of tert-butylmethylether (8 mL) and ethyl acetate (4 mL) at 50° C. for 10 minutes, filtered, washed with tert-butylmethylether (10 mL) and dried in vacuo at 40° C. to give 8′-fluoro-5′-methoxy-1′H-spiro[cyclohexane-1,4′-quinazolin]-2′(3′H)-one (900 mg, 70%) as a light-brown solid, purity (97.3%).

1. temperaturecooled to 35° C.
2. customquenched into water (400 mL)
3. filtrationThe crude product was filtered
4. washwashed with water (100 mL)
5. additionThe isolated solid was slurred in a mixture of tert-butylmethylether (8 mL) and ethyl acetate (4 mL) at 50° C. for 10 minutes
6. filtrationfiltered
7. washwashed with tert-butylmethylether (10 mL)
8. customdried in vacuo at 40° C.