反应详情

温度

22.5 °C

4-[3-[[6,7-Bis(2-methoxyethoxy]-4-quinazolinyl]amino]phenyl]-2-methyl-3-butyn-2-ol, prepared above (5.0 g, 11 mmol), anhydrous solid sodium hydroxide (44 mg, 11 mmol) and 2-methoxyethanol (50 mL) were stirred together and heated at reflux for 47 hours. The reaction mixture was cooled to 20-25° C. and concentrated hydrochloric acid (1.1 mL) was added. The resultant mixture was granulated at 20-25° C. for 1 hour to establish crystallization. The title product crystals were isolated by filtration, washed with 2-methoxyethanol (10 mL) and dried under vacuum at 45-50° C. to remove 2-methoxyethanol. Yield (3.73 g, 78%).

1. temperatureheated
2. temperatureat reflux for 47 hours
3. customcrystallization