反应详情

温度

70 °C

Potassium carbonate (147 mg, 1.06 mmol) was added to a solution of methyl (4′-hydroxy-2-nitro-1,1′-biphenyl-4-yl)acetate (203 mg, 0.71 mmol) obtained in Example (37-1) and tert-butyl 6-(bromomethyl)-2-[(tert-butoxycarbonyl)oxy]-3-(trifluoromethyl)benzoate (330 mg, 0.781 mmol) obtained in Example (28-5) in acetone (15 ml), and the mixture was stirred at 70° C. for 8 hours. The reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was successively washed with water and a saturated aqueous NaCl solution and dried with anhydrous sodium sulfate. The residue obtained by removing the solvent under reduced pressure was subjected to silica gel column chromatography (eluting solvent: hexane/ethyl acetate=4/1) to give crude tert-butyl 2-[(tert-butoxycarbonyl)oxy]-6-[({4′-[(methoxycarbonyl)methyl]-2′-nitro-1,1′-biphenyl-4-yl}oxy)methyl]-3-(trifluoromethyl)benzoate.

1. extractionextracted with ethyl acetate
2. washThe organic layer was successively washed with water
3. dry with materiala saturated aqueous NaCl solution and dried with anhydrous sodium sulfate
4. customThe residue obtained
5. customby removing the solvent under reduced pressure
6. washwas subjected to silica gel column chromatography (eluting solvent: hexane/ethyl acetate=4/1)