反应详情

The compound (150 mg, 0.21 mmol) obtained in Example 94b was dissolved in ethanol (0.5 mL), a 4 N hydrochloric acid-1,4-dioxane solution (5.1 mL, 20.6 mmol) was added, and the mixture was stirred at room temperature under a nitrogen atmosphere for 6 hours. After the reaction was completed, the solvent was evaporated under reduced pressure. Ethyl acetate was added under ice cooling, a saturated aqueous sodium hydrogencarbonate solution was further added to neutralize the mixture and separate the layers. The resulting organic layer was separated, washed with saturated sodium chloride solution, and then dried with anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate:methanol, 10:1, v/v) to give the title compound (98 mg; yield, 76%) as a colorless oily substance.

1. customthe solvent was evaporated under reduced pressure
2. additionEthyl acetate was added under ice cooling
3. additiona saturated aqueous sodium hydrogencarbonate solution was further added
4. customseparate the layers
5. customThe resulting organic layer was separated
6. washwashed with saturated sodium chloride solution
7. dry with materialdried with anhydrous sodium sulfate
8. customthe solvent was evaporated under reduced pressure
9. customThe residue was purified by NH silica gel column chromatography (ethyl acetate