反应详情

2-[(4-{2-[(4′-Fluorobiphenyl-4-yl)oxy]-1-hydroxyethyl}-1,3-thiazol-2-yl)thio]-2-methylpropionic acid tert-butyl ester (877 mg) obtained in Example 2-2 was dissolved in methylene chloride (3 mL), trifluoroacetic acid (3 mL) was added and the mixture was stirred at room temperature overnight. The solvent was evaporated and the obtained residue was dissolved in ethyl acetate (30 mL), washed successively with water and saturated aqueous sodium chloride solution, and dried over anhydrous sodium sulfate. The solvent was evaporated and the obtained residue was applied to column chromatography (Moritex Corporation Purif Pack SI 60 μm size 200 was used. elution solvent: hexane/ethyl acetate=7/3→0/10). The solvent was evaporated from the obtained fraction containing the object product to give a white solid. This was dissolved in a mixed solvent of hexane and ethyl acetate with heating, and the mixture was cooled to allow precipitation of a solid to give the title compound (450.6 mg).

1. customThe solvent was evaporated
2. dissolutionthe obtained residue was dissolved in ethyl acetate (30 mL)
3. washwashed successively with water and saturated aqueous sodium chloride solution
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was evaporated
6. washthe obtained residue was applied to column chromatography (Moritex Corporation Purif Pack SI 60 μm size 200 was used. elution solvent: hexane/ethyl acetate=7/3→0/10)
7. customThe solvent was evaporated from the obtained fraction
8. additioncontaining the object product
9. customto give a white solid
10. temperaturewith heating
11. temperaturethe mixture was cooled
12. customprecipitation of a solid