反应详情

温度

90 °C

36 mg of 3-methoxyphenylboronic acid, 55 mg of sodium carbonate and 30 mg polymer supported bis(acetato)triphenylphosphine palladium(II) were added to 2.5 mL of N,N-dimethylacetamide solution containing 70 mg of methyl 2-(benzamido)-4-bromobenzoate, and stirred at 90° C. for 11 hours. After the reaction mixture was cooled to room temperature, insoluble were removed by filtration and ethyl acetate and 1.2 mol/L hydrochloric acid were added. The organic layer was separated and dried over anhydrous magnesium sulfate after washed with 1.0 mol/L hydrochloric acid, a saturated sodium hydrogen carbonate aqueous solution and a saturated sodium chloride aqueous solution sequentially, and one solvent was evaporated under reduced pressure, 1.0 mL of 1.0 mol/L aqueous sodium hydroxide and 2.0 mL of ethanol were added to the obtained residue and stirred at room temperature for 1 hour. 0.6 mol/L hydrochloric acid was added to the reaction mixture and a solid substance was separated by filtration to obtain 18 mg of 2-(benzamido)-4-(3-methoxyphenyl)benzoic acid as white solid.

1. temperatureAfter the reaction mixture was cooled to room temperature
2. custominsoluble were removed by filtration and ethyl acetate and 1.2 mol/L hydrochloric acid
3. additionwere added
4. customThe organic layer was separated
5. dry with materialdried over anhydrous magnesium sulfate
6. washafter washed with 1.0 mol/L hydrochloric acid
7. customa saturated sodium hydrogen carbonate aqueous solution and a saturated sodium chloride aqueous solution sequentially, and one solvent was evaporated under reduced pressure, 1.0 mL of 1.0 mol/L aqueous sodium hydroxide and 2.0 mL of ethanol
8. additionwere added to the obtained residue
9. stirringstirred at room temperature for 1 hour
10. addition0.6 mol/L hydrochloric acid was added to the reaction mixture
11. customa solid substance was separated by filtration