反应详情

温度

137.5 °C

4-[3-[[6,7-Bis(2-methoxyethoxy]-4-quinazolinyl]amino]phenyl]-2-methyl-3-butyn-2-ol, prepared above (20.0 g, 44.3 mmol), anhydrous solid sodium hydroxide (260 mg, 6.5 mmol) and propan-2-ol (200 mL) were stirred together and heated in a pressure vessel at 135-140° C. for 23 hours. The reaction mixture was cooled to 60-65° C. and concentrated hydrochloric acid (4.8 mL) was added. The resultant mixture was granulated overnight at 20-25° C. to establish crystallization. The mixture was treated with water (10 mL) and stirred at 58-60° C. for 21 hours, cooled to 15-20° C. and granulated for 2 hours. The title product crystals were isolated by filtration, washed with propan-2-ol (2×30 mL) and dried under vacuum at 45-50° C. to remove propan-2-ol. Yield (17.6 g, 92%).

1. temperatureThe reaction mixture was cooled to 60-65° C.
2. customcrystallization
3. additionThe mixture was treated with water (10 mL)
4. stirringstirred at 58-60° C. for 21 hours
5. temperaturecooled to 15-20° C.