反应详情

温度

110 °C

To 5 mL of N,N-dimethylacetamide solution containing 0.60 g of tert-butyl 4-bromo-2-nitrobenzoate, 0.37 mL of 3-vinylanisole, 0.47 mL of triethylamine and 0.11 g of palladium acetate were added at room temperature and stirred under nitrogen atmosphere at 110° C. for 4 hours. Ethyl acetate and water were added after the reaction mixture was cooled to room temperature. The organic layer was separated and dried over anhydrous magnesium sulfate after washed with 10% citric acid aqueous solution and a saturated sodium chloride aqueous solution sequentially, and the solvent was evaporated under reduced pressure. The obtained residue was purified with silica gel column chromatography [PSQ100B (spherical) manufactured by Fuji Silysia Chemical Ltd., eluent; hexane:ethyl acetate=10:1] to obtain 0.20 g of tert-butyl 4-((E)-2-(3-methoxyphenyl)vinyl)-2-nitrobenzoate a pale yellow solid.

1. additionwere added at room temperature
2. temperaturewas cooled to room temperature
3. customThe organic layer was separated
4. dry with materialdried over anhydrous magnesium sulfate
5. washafter washed with 10% citric acid aqueous solution
6. customa saturated sodium chloride aqueous solution sequentially, and the solvent was evaporated under reduced pressure
7. customThe obtained residue was purified with silica gel column chromatography [PSQ100B (spherical) manufactured by Fuji Silysia Chemical Ltd., eluent; hexane:ethyl acetate=10:1]