反应详情

To 15 mL of toluene solution containing 1.5 g of tert-butyl 4-chloro-2-nitrobenzoate, 1.1 g of 2,4-difluorophenylboronic acid, 2.3 g of cesium carbonate, 27 mg of palladium acetate and 25 mg of 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl were added sequentially, and the resulting mixture was heated to reflux under nitrogen atmosphere for 8 hours. After the reaction mixture was cooled to room temperature, insoluble were removed by filtration and added a saturated sodium hydrogen carbonate aqueous solution. 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. Hexane and diisopropyl ether were added to the obtained residue and a solid substance was separated by filtration to obtain 0.95 g of tert-butyl 4-(2,4-difluorophenyl)-2-nitrobenzoate as white solid.

1. additionwere added sequentially
2. temperaturethe resulting mixture was heated
3. temperatureto reflux under nitrogen atmosphere for 8 hours
4. custominsoluble were removed by filtration
5. additionadded a saturated sodium hydrogen carbonate aqueous solution
6. customThe organic layer was separated
7. dry with materialdried over anhydrous magnesium sulfate
8. washafter washed with 10% citric acid aqueous solution
9. customa saturated sodium chloride aqueous solution sequentially, and the solvent was evaporated under reduced pressure
10. additionHexane and diisopropyl ether were added to the obtained residue
11. customa solid substance was separated by filtration