反应详情

温度

70 °C

After tripotassium phosphate (127 mg, 0.60 mmol), palladium acetate (8 mg, 0.04 mmol) and 2-(dicyclohexylphosphino)-2′,6′-dimethoxy-1,1′-biphenyl (S-PHOS) (16 mg, 0.04 mmol) were added to a solution of methyl (4-chloro-2-methoxyphenyl)acetate (43 mg, 0.2 mmol) obtained in Example (24-1) and tert-butyl 2-hydroxy-{[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenoxy]methyl}-3-(trifluoromethyl)benzoate (100 mg, 0.2 mmol) obtained in Example (22-4) in toluene (2.0 ml), the mixture was stirred at 70° C. for 4 hours. After the temperature of the reaction mixture was returned to room temperature, the mixture was poured into water and extracted with ethyl acetate (three times). The organic layer was successively washed with water (twice) and a saturated aqueous NaCl solution and dried with anhydrous sodium sulfate. The residue obtained by removing the solvent under reduced pressure was purified by silica gel column chromatography (eluting solvent: n-hexane/ethyl acetate=2/1) to give tert-butyl 2-hydroxy-6-[({4′-[(methoxycarbonyl)methyl]-3′-methoxy-1,1′-biphenyl-4-yl}oxy)methyl]-3-(trifluoromethyl)benzoate (100 mg, yield: 60%).

1. customwas returned to room temperature
2. extractionextracted with ethyl acetate (three times)
3. washThe organic layer was successively washed with water (twice) and a saturated aqueous NaCl solution
4. dry with materialdried with anhydrous sodium sulfate
5. customThe residue obtained
6. customby removing the solvent under reduced pressure
7. customwas purified by silica gel column chromatography (eluting solvent: n-hexane/ethyl acetate=2/1)