反应详情

温度

100 °C

Phenol (0.029 mL), cesium carbonate (0.11 g), 2,2,6,6-tetramethylheptane-3,5-dione (3.4 μL), and copper(I) chloride (8.2 mg) were added to a 1-methyl-2-pyrrolidone (0.60 mL) solution of tert-butyl 2-(2-(benzyloxy)-5-iodobenzamido)-4-phenylbenzoate (0.10 g), followed by stirring under a nitrogen atmosphere at 100° C. for 2 hours. The reaction mixture was cooled to room temperature, and then 2,2,6,6-tetramethylheptane-3,5-dione (3.4 μL) and copper(I) chloride (8.2 mg) were added thereto, followed by stirring under a nitrogen atmosphere at 100° C. for 2 hours. The reaction mixture was cooled to room temperature, and then a 10% aqueous solution of citric acid and ethyl acetate were added thereto. The organic layer was separated, washed with a saturated aqueous solution of sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography [eluent: 100-95% hexane/ethyl acetate] to obtain 0.049 g of tert-butyl 2-(2-(benzyloxy)-5-phenoxybenzamido)-4-phenylbenzoate (0.049 g).

1. temperatureThe reaction mixture was cooled to room temperature
2. stirringby stirring under a nitrogen atmosphere at 100° C. for 2 hours
3. temperatureThe reaction mixture was cooled to room temperature
4. customThe organic layer was separated
5. washwashed with a saturated aqueous solution of sodium chloride
6. dry with materialdried over anhydrous magnesium sulfate
7. customthe solvent was evaporated under reduced pressure
8. customThe obtained residue was purified by silica gel column chromatography [eluent: 100-95% hexane/ethyl acetate]