反应详情

温度

120 °C

To a solution of 1-Bromo-4-methyl-2-nitro-benzene (0.76 g, 3.5 mmol), 1-methoxy-4-vinyl-benzene (0.59 g, 4.4 mmol), triethylamine (0.88 g, 8.8 mmol), tri-o-tolylphosphine (0.022 g) and palladium acetate (0.008 g) in N,N-dimethylformamide (7 mL) was placed in a high-pressure tube and purged with nitrogen for 10 mins. The tube was sealed and heated at 120° C. for 16 hours. The mixture was partitioned with water and ethyl acetate adjusting the pH to 3. The organic layer was washed with brine, dried (sodium sulfate) and filtered through a plug of silica. The filtrate was evaporated under vacuum and the residue was triturated with hexane/ethyl acetate (9:1) to provide the title compound (0.55 g, 58%).

1. custompurged with nitrogen for 10 mins
2. customThe tube was sealed
3. customThe mixture was partitioned with water and ethyl acetate adjusting the pH to 3
4. washThe organic layer was washed with brine
5. dry with materialdried (sodium sulfate)
6. filtrationfiltered through a plug of silica
7. customThe filtrate was evaporated under vacuum
8. customthe residue was triturated with hexane/ethyl acetate (9:1)