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, 0.50 mL of 4-phenyl-1-butene and 0.46 mL of triethylamine, and the resulting mixture was heated to reflux under nitrogen atmosphere for 4 hours and 30 minutes. 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 5 hours and 30 minutes. After cooled to room temperature, the reaction mixture was purified with silica gel column chromatography [eluent; hexane:ethyl acetate=30:1] to obtain 0.35 g of tert-butyl 2-nitro-4-(4-phenyl-1-butenyl)benzoate.

1. temperaturethe resulting mixture was heated
2. temperatureto reflux under nitrogen atmosphere for 4 hours and 30 minutes
3. temperaturethe resulting mixture was heated
4. temperatureto reflux for 5 hours and 30 minutes
5. temperatureAfter cooled to room temperature
6. customthe reaction mixture was purified with silica gel column chromatography [eluent; hexane:ethyl acetate=30:1]