反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
51 mg of benzofuran-2-boronic acid, 55 mg of sodium carbonate and 30 mg of 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 22 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 and a saturated sodium chloride aqueous solution sequentially, and the 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 11 mg of 2-(benzamido)-4-(benzofuran-2-yl)benzoic acid as whine solid.
WORKUP
后处理
- temperatureAfter the reaction mixture was cooled to room temperature
- custominsoluble were removed by filtration and ethyl acetate and 1.2 mol/L hydrochloric acid
- additionwere added
- customThe organic layer was separated
- dry with materialdried over anhydrous magnesium sulfate
- washafter washed with 1.0 mol/L hydrochloric acid
- customa saturated sodium chloride aqueous solution sequentially, and the solvent was evaporated under reduced pressure
- addition1.0 mL of 1.0 mol/L aqueous sodium hydroxide and 2.0 ml, of ethanol were added to the obtained residue
- stirringstirred at room temperature for 1 hour
- addition0.6 mol/L hydrochloric acid was added to the reaction mixture
- customa solid substance was separated by filtration