反应详情

温度

55 °C

In a 100 mL volume glass vessel equipped with a stirrer and a thermometer were placed 15.0 g (55.8 mmol) of 6-methoxy-7-(3-chloropropoxy)quinazolin-4-one prepared by procedures similar to those of Reference Example V-1, 13.85 g (163 mmol) of piperidine, and 27.4 mL (113.6 mmol) of aqueous sodium hydroxide solution (4.0 mol/L). The resulting mixture was stirred at 55° C. for 5 hours. After the reaction was complete, the reaction mixture was cooled to room temperature and placed under reduced pressure to distill unreacted piperidine off. To the residue was added 18.9 mL (113.4 mmol) of hydrochloric acid (6.0 mol/L), and the mixture was cooled to 0° C. The precipitated crystalline product was collected by filtration and dried at 60° C. under reduced pressure, to give 13.5 g (isolated yield: 76.3%) of 6-methoxy-7-(3-piperidino-propoxy)quinazolin-4-one.

1. customIn a 100 mL volume glass vessel equipped with a stirrer
2. temperaturethe reaction mixture was cooled to room temperature
3. distillationto distill unreacted piperidine off
4. temperaturethe mixture was cooled to 0° C
5. filtrationThe precipitated crystalline product was collected by filtration
6. customdried at 60° C. under reduced pressure