反应详情

[4′-(1-{4-[3-(t-Butyl-dimethyl-silanyloxy)-4,4-dimethyl-pentyl]-3-methyl-phenyl}-1-ethyl-propyl)-2′-methyl-biphenyl-3-yl]-acetic acid methyl ester (Example 66-(1); 36 mg, 0.057 mmol) was dissolved in dichloromethane/trifluoroacetic acid=1/5 (1 mL), and the solution was stirred at room temperature for three hours. The reaction mixture was concentrated under reduced pressure, and then the residue was purified by silica gel chromatography (hexane only to hexane/ethyl acetate=1/1). The product was dissolved in methanol/tetrahydrofuran=1/1 (1 mL). A 1 N sodium hydroxide aqueous solution (0.1 mL) was added, and the mixture was stirred at room temperature for one hour. A 30% sodium dihydrogenphosphate aqueous solution (0.3 mL) was added to the reaction mixture, and then the reaction mixture was concentrated under reduced pressure. The residue was purified by preparative TLC (hexane/ethyl acetate=1/1) to give the title compound (23 mg, 80%).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. customthe residue was purified by silica gel chromatography (hexane only to hexane/ethyl acetate=1/1)
3. dissolutionThe product was dissolved in methanol/tetrahydrofuran=1/1 (1 mL)
4. additionA 1 N sodium hydroxide aqueous solution (0.1 mL) was added
5. stirringthe mixture was stirred at room temperature for one hour
6. additionA 30% sodium dihydrogenphosphate aqueous solution (0.3 mL) was added to the reaction mixture
7. concentrationthe reaction mixture was concentrated under reduced pressure
8. customThe residue was purified by preparative TLC (hexane/ethyl acetate=1/1)