反应详情

To a solution of Example 9A (5.4 g, 0.022 mol) in dichloromethane at −78° C. was added a solution of BBr3 (0.066 mol) drop wise and the reaction mixture was stirred overnight while warming up to room temperature. The mixture was poured into ice and then stirred at room temperature for 24 hours. The organic layer was washed with brine, dried over magnesium sulfate and filtered. The filtrate was concentrated under vacuum to give 3.5 g of product as an off-white solid (70% yield). 1H NMR (300 MHz, CDCl3) δ ppm 6.59 (dd, J=8.82, 2.94 Hz, 1H) 6.67 (d, J=2.57 Hz, 1H) 6.88 (d, J=3.68 Hz, 1H) 7.07 (d, J=8.82 Hz, 1H) 7.19 (d, J=3.68 Hz, 1H). MS (ESI) M/z 227.9 (M+H)+.

1. additionThe mixture was poured into ice
2. stirringstirred at room temperature for 24 hours
3. washThe organic layer was washed with brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationThe filtrate was concentrated under vacuum