反应详情

A mixture of the compound obtained in Example 66 (391 mg, 0.80 mmol), 2-bromoacetamide (132 mg, 0.96 mmol), potassium carbonate (265 mg, 1.92 mmol) and DMF (5 mL) was stirred at room temperature for 2 days. To the reaction mixture was added water (15 mL), and the mixture was extracted with ethyl acetate (15 mL×3). The organic layer was washed with water (5 mL×3), saturated sodium chloride solution (5 mL), successively, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The concentrate was subjected to column chromatography (silica gel 10 g, ethyl acetate/methanol=1/0 to 9/1), and the desired fraction was concentrated under reduced pressure to give the titled compound (357 mg, 0.65 mmol, Yield 82%) as a colorless oily substance.

1. extractionthe mixture was extracted with ethyl acetate (15 mL×3)
2. washThe organic layer was washed with water (5 mL×3), saturated sodium chloride solution (5 mL)
3. dry with materialsuccessively, dried over anhydrous sodium sulfate
4. concentrationconcentrated under reduced pressure
5. concentrationthe desired fraction was concentrated under reduced pressure