反应详情

To a 0.55M solution of 2-chloro-8-methoxyquinazoline in DCM was added boron tribromide (2.2 eq. of a 1.0 M solution in DCM) over 5 minutes at 0° C. The reaction mixture was stirred at ambient temperature for 22 hours, and then cooled to −5° C. for 30 minutes. The precipitate was collected by vacuum filtration and then stirred in ice water for 30 minutes. The solid was collected by vacuum filtration and rinsed with 2-propanol. The off-white solid was dried in a desiccator to give the desired product in 79% yield. ES/MS m/z 181 (MH+).

1. temperaturecooled to −5° C. for 30 minutes
2. filtrationThe precipitate was collected by vacuum filtration
3. stirringstirred in ice water for 30 minutes
4. filtrationThe solid was collected by vacuum filtration
5. washrinsed with 2-propanol
6. customThe off-white solid was dried in a desiccator