反应详情

温度

140 °C

10.00 kg (22.06 mol) of 1-[(4-methylquinazolin-2-yl)methyl]-3-methyl-7-(2-butin-1-yl)-8-bromoxanthine, 12.59 kg (33.09 mol) of 3-(phthalimido)piperidine D-tartrate and 17.5 liters of N-methyl-2-pyrrolidone are initially charged in the reactor. The reactor contents are heated to 140° C. After the temperature has been attained, 11.41 kg (88.24 mol) of diisopropylethylamine are metered in within 20 minutes. The feed vessel is flushed with 2.5 liters of N-methyl-2-pyrrolidone and the reaction mixture is subsequently stirred at 140° C. for 2 hours. After the reaction has ended, the reaction mixture is cooled to 60° C. and diluted with 80 liters of methanol. The resulting suspension is stirred at 50° C. for 30 minutes, then cooled to 23° C. and stirred for a further 30 minutes. Subsequently, the product is centrifuged off and washed 3 times with 20 liters each time of methanol. Drying is effected at 45° C. in a drying cabinet under inertization.

1. customare metered in within 20 minutes
2. customThe feed vessel is flushed with 2.5 liters of N-methyl-2-pyrrolidone
3. temperaturethe reaction mixture is cooled to 60° C.
4. additiondiluted with 80 liters of methanol
5. stirringThe resulting suspension is stirred at 50° C. for 30 minutes
6. temperaturecooled to 23° C.
7. stirringstirred for a further 30 minutes
8. washwashed 3 times with 20 liters each time of methanol
9. customDrying
10. customis effected at 45° C. in a drying cabinet under inertization