反应详情

温度

-78 °C

To 2-(3-methoxyphenyl)quinazolin-4(3H)-one (11.6 g, 45.98 mmole) was added of CH2Cl2 (120 mL) and the mixture was cooled to −78° C. Then, a 1 M solution of BBr3 in CH2Cl2 (60 mL, 60.0 mmol) was added drop wise and the reaction was stirred at −78° C. for 1 h and then ambient temperature for 3 h. The reaction was re-cooled to −78° C. and cautiously quenched with MeOH (20 mL). The ice bath was removed and the system allowed to stir at ambient temperature for 0.5 h. The pH was adjusted to 7 with 10% w/w NaHCO3 solution. The solid was filtered, washed with ether, dried and then azeotroped from toluene (3×) and dried under high vacuum overnight to give 2-(3-hydroxyphenyl)quinazolin-4(3H)-one. (11.0 g, mmol, 100%).

1. waitambient temperature for 3 h
2. temperatureThe reaction was re-cooled to −78° C.
3. customcautiously quenched with MeOH (20 mL)
4. customThe ice bath was removed
5. stirringto stir at ambient temperature for 0.5 h
6. filtrationThe solid was filtered
7. washwashed with ether
8. customdried
9. customazeotroped from toluene (3×)
10. customdried under high vacuum overnight