反应详情

To a solution of EXAMPLE 412A (1.5 g, 6.8 mmol) and triphenyl phosphine (1.9 g, 7.2 mmol) in dimethylformamide (20 ml) was added bromine (1.1 g, 6.8 mmol) through a syringe. After the addition, the reaction mixture was stirred at room temperature for additional 15 minutes, and partitioned between water (100 ml) and ethyl acetate (200 ml). The organic phase was washed with brine and concentrated. The residue was purified by flash chromatography (2.6% ethyl acetate in hexane) to provide the title compound. MS (DCI/NH4) m/z 282 (M+H)+.

1. additionAfter the addition
2. custompartitioned between water (100 ml) and ethyl acetate (200 ml)
3. washThe organic phase was washed with brine
4. concentrationconcentrated
5. customThe residue was purified by flash chromatography (2.6% ethyl acetate in hexane)