反应详情

19 mg of palladium acetate (II) was added to 5 mL of toluene solution containing 0.50 g of tert-butyl 4-bromo-2-nitrobenzoate, 50 mg of tri(o-tolyl)phosphine, 0.44 mL of allylbenzene and 0.46 mL of triethylamine, and the resulting mixture was heated to reflux under nitrogen atmosphere for 2 hours. After the reaction mixture was cooled to room temperature, 20 mg of palladium acetate (II) was added and the resulting mixture was heated to reflux for 7 hours. After the reaction mixture was cooled to room temperature, Insoluble were removed by filtration, and the solvent was evaporated under reduced pressure. The obtained residue was purified with silica gel column chromatography [eluent; hexane:ethyl acetate=30:1] to obtain 0.31 g of tert-butyl 2-nitro-4-(3-phenyl-1-propenyl)benzoate.

1. temperaturethe resulting mixture was heated
2. temperatureto reflux under nitrogen atmosphere for 2 hours
3. temperaturethe resulting mixture was heated
4. temperatureto reflux for 7 hours
5. temperatureAfter the reaction mixture was cooled to room temperature
6. customInsoluble were removed by filtration
7. customthe solvent was evaporated under reduced pressure
8. customThe obtained residue was purified with silica gel column chromatography [eluent; hexane:ethyl acetate=30:1]