反应详情

温度

80 °C

A mixture of (S)-tert-butyl (1-(4-bromophenyl)ethyl)carbamate (D1) (9.20 g, 27.3 mmol), 1,3-bis(diphenylphosphino)-propane (2.25 g, 5.46 mmol), palladium (II) acetate (1.22 g, 5.46 mmol), and triethylamine (11.5 ml, 81.9 mmol) in N,N-dimethylformamide/methanol (60 ml/60 ml) was stirred at 80° C. overnight under carbon monoxide atmosphere. After cooling to room temperature, the mixture was diluted with ether (300 ml) and washed with water (3×100 ml). The organic layer was dried over Na2SO4 and evaporated in vacuo. The residue was purified by flash chromatography on silica gel eluting with a mixture petroleum ether/ethyl acetate 5:1 to afford the title compound (D2) (6.72 g) as white solid.

1. temperatureAfter cooling to room temperature
2. washwashed with water (3×100 ml)
3. dry with materialThe organic layer was dried over Na2SO4
4. customevaporated in vacuo
5. customThe residue was purified by flash chromatography on silica gel eluting with a mixture petroleum ether/ethyl acetate 5:1