反应详情

A solution of the compound (451 mg, 0.82 mmol) obtained in Example 71-1) and tetrabutylammonium fluoride (1 M tetrahydrofuran solution, 0.98 mL) in tetrahydrofuran (4 mL) was stirred at room temperature for 18 h. Saturated aqueous ammonium chloride was added to the reaction mixture, the mixture was extracted with dichloromethane, and the organic layer was washed with saturated sodium chloride solution and dried with anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel chromatography (Isco Combiflash, 12 g, methanol:ethyl acetate=0:100 to 40:60, gradient) to obtain the title compound (321 mg, 90%) as a colorless solid.

1. extractionthe mixture was extracted with dichloromethane
2. washthe organic layer was washed with saturated sodium chloride solution
3. dry with materialdried with anhydrous sodium sulfate
4. filtrationAfter filtration
5. concentrationthe filtrate was concentrated under reduced pressure
6. customthe residue was purified by silica gel chromatography (Isco Combiflash, 12 g, methanol:ethyl acetate=0:100 to 40:60, gradient)