反应详情

The compound (0.31 g, 1.66 mmol) obtained in Step (ii) was dissolved in THF (10 ml), and thereto were added at 0° C. dimethylamine (2M THF solution, 2.62 ml, 5.24 mmol) and sodium triacetoxy borohydride (0.56 g, 2.62 mmol), and the mixture was stirred at room temperature for 20 hours. The mixture was cooled to 0° C., and thereto was added a saturated aqueous sodium hydrogencarbonate solution, and the mixture was extracted three times with chloroform/ethanol=3/1. The extract was dried over magnesium sulfate, concentrated, and purified by silica gel column (chloroform/methanol/28% aqueous ammonia=100/5/0 to 100/5/1) to give the title compound (0.28 g, 0.57 mmol) as a white solid. Yield: 87%.

1. temperatureThe mixture was cooled to 0° C.
2. extractionthe mixture was extracted three times with chloroform/ethanol=3/1
3. dry with materialThe extract was dried over magnesium sulfate
4. concentrationconcentrated
5. custompurified by silica gel column (chloroform/methanol/28% aqueous ammonia=100/5/0 to 100/5/1)