反应详情

To a solution of N-(3-{[2-(acetylamino)-1,3-benzothiazol-6-yl]oxy}phenyl)-2,2,2-trifluoroacetamide (10.0 g, 25.3 mmol) in tetrahydrofuran (50 mL) were added methanol (25 mL), water (25 mL) and lithium hydroxide monohydrate (1.50 g, 35.7 mmol), and the mixture was stirred at room temperature for 1 hr. To the reaction mixture were added water (200 mL) and ethyl acetate (250 mL), and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography (hexane/ethyl acetate=20/80→0/100), and triturated with ethyl acetate/hexane to give the title compound (3.10 g, 41%) as a yellow solid.

1. extractionthe mixture was extracted with ethyl acetate
2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
3. concentrationthe filtrate was concentrated under reduced pressure
4. customThe residue was purified by silica gel chromatography (hexane/ethyl acetate=20/80→0/100)
5. customtriturated with ethyl acetate/hexane