反应详情

In 20 ml of dichloromethane, was dissolved 298 mg of the compound obtained in Example 16. To the resulting solution, was added 3.0 ml of triethylamine. To the obtained mixture, 0.46 ml of acetyl chloride was added under cooling with ice and stirring. The mixture was stirred at 0° C. to room temperature for 18 hours. The obtained mixture was poured into a saturated aqueous solution of sodium hydrogensulfate and extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium hydrogencarbonate and saturated brine and subsequently dried over magnesium sulfate. The solvent was removed under reduced pressure, and the obtained crude product was purified by silica gel column chromatography to afford 260 mg (78%) of the title compound.

1. temperatureunder cooling with ice
2. stirringThe mixture was stirred at 0° C. to room temperature for 18 hours
3. extractionextracted with ethyl acetate
4. washThe organic layer was washed with a saturated aqueous solution of sodium hydrogencarbonate and saturated brine
5. dry with materialsubsequently dried over magnesium sulfate
6. customThe solvent was removed under reduced pressure
7. customthe obtained crude product
8. customwas purified by silica gel column chromatography