反应详情

温度

160 °C

A mixture of compound 41 (0.35 g, 0.99 mmol), Pd(OAc)2 (33 mg, 0.15 mmol), (cyclohexyl)3PBF4 (110 mg, 0.30 mmol), and K2CO3 (138 mg, 0.10 mmol) in DMA (3 mL) was purged with N2 for 20 minutes and then heated at 160° C. for 3 hours. The reaction was cooled to room temperature and diluted with ethyl acetate. The organic layer was washed with water and brine, dried over sodium sulfate and concentrated. Purification by flash chromatography (ethyl acetate/hexane) gave compound 42 as a yellow solid (110 mg, 41%). LCMS-ESI (POS), M/Z, M+1: Found 267.1, Calculated 267.2.

1. customwas purged with N2 for 20 minutes
2. temperatureThe reaction was cooled to room temperature
3. additiondiluted with ethyl acetate
4. washThe organic layer was washed with water and brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customPurification by flash chromatography (ethyl acetate/hexane)