反应详情

温度

90 °C

To a cooled (0° C.) suspension of 6-iodoquinazolin-4-ol (107.6 g, 396 mmol) and DIEA (138 mL, 791 mmol) in dichloroethane (600 mL) was added POCl3 (44.25 mL, 475 mmol). After heating to 90° C. for 16 hours, the reaction mixture was cooled to room temperature and the crystals (73.8 g) collected by filtration. The filtrate was concentrated under reduced pressure and azeotroped twice with toluene. The solids (8.3 g) were triturated with isopropanol (450 mL) and cooled in an ice bath before collecting by filtration and drying under high vacuum. The two solids were combined to provide the product (82.1 g, 71%) as white solid.

1. temperatureTo a cooled
2. temperaturethe reaction mixture was cooled to room temperature
3. filtrationthe crystals (73.8 g) collected by filtration
4. concentrationThe filtrate was concentrated under reduced pressure
5. customazeotroped twice with toluene
6. customThe solids (8.3 g) were triturated with isopropanol (450 mL)
7. temperaturecooled in an ice bath
8. filtrationbefore collecting by filtration
9. customdrying under high vacuum