反应详情

To tert-butyl 5-bromo-2-fluorobenzoate (1.26 g) in dimethoxyethane (22.9 ml) solution, tris(dibenzylideneacetone)dipalladium (0.10 g), 2-(di-tert-butylphosphino)-2′-methylbiphenyl (0.14 g), tripotassium phosphate (1.07 g), and 1-nitropropane (0.82 ml) were added, the mixture was stirred at room temperature for 1 minute, then the mixture was stirred under heating and reflux for 15 hours. The insoluble compound was filtered out, then the filtrate was concentrated. The residue was purified by silica gel column chromatography (hexane/ethyl acetate, ethyl acetate: 0 to 10%) to obtain the title compound (392 mg).

1. stirringthe mixture was stirred
2. temperatureunder heating
3. temperaturereflux for 15 hours
4. filtrationThe insoluble compound was filtered out
5. concentrationthe filtrate was concentrated
6. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate, ethyl acetate: 0 to 10%)