反应详情

To a solution of the title compound of Step F in dichloromethane (2.2 ml) at room temperature was added boron tribromide (1M in dichloromethane, 1.5 ml, 1.5 mmol). The reaction mixture was stirred at room temperature for about two hours, and quenched with water (20 ml). After stirring for about 15 minutes, the solution was extracted with dichloromethane (3×15 ml). The combined organic extracts were washed with brine (50 ml), treated with activated carbon, filtered through diatomaceous earth, dried and concentrated to give the title compound (163 mg) as an off-white solid which was used in the next step without further purification. MS (APCI−) Calc: 457.0, found: 456.0 (M−1).

1. customquenched with water (20 ml)
2. stirringAfter stirring for about 15 minutes
3. extractionthe solution was extracted with dichloromethane (3×15 ml)
4. washThe combined organic extracts were washed with brine (50 ml)
5. additiontreated with activated carbon
6. filtrationfiltered through diatomaceous earth
7. customdried
8. concentrationconcentrated