反应详情

温度

100 °C

N-(4-{[7-(Benzyloxy)-6-methoxy-4-quinazolinyl]oxy}-2-chlorophenyl)-N′-propylurea (42.2 g) was dissolved in trifluoroacetic acid (200 ml). Methanesulfonic acid (11.1 ml) was then added to the solution, and the mixture was stirred at 100° C. for 4 hr. The reaction solution was cooled to room temperature, and trifluoroacetic acid was removed by distillation under the reduced pressure. Chloroform and methanol were added to the mixture as the residue, followed by extraction with a 10% aqueous sodium hydroxide solution three times. The aqueous layer was neutralized with concentrated hydrochloric acid to precipitate a solid. The solid was washed with water, methanol, and ether in that order, and was then dried in vacuo through a vacuum pump to give 20.7 g (yield 60%) of the title compound.

1. temperatureThe reaction solution was cooled to room temperature
2. customtrifluoroacetic acid was removed by distillation under the reduced pressure
3. additionChloroform and methanol were added to the mixture as the residue
4. extractionfollowed by extraction with a 10% aqueous sodium hydroxide solution three times
5. customto precipitate a solid
6. washThe solid was washed with water, methanol, and ether in that order
7. customwas then dried in vacuo through a vacuum pump