反应详情

温度

60 °C

Under an argon atmosphere, to a solution of 2-amino-3-benzyl-5-(4-methoxy-2-vinylphenyl)-6-vinylpyrazine (9) (100 mg, 292 μmol) in anhydrous pyridine (20 mL) were successively added 4-(dimethylamino)pyridine (DMAP) (3.0 mg, 25 μmol) and acetyl chloride (65.0 μL, 911 μmol) at room temperature. The mixture was heated at 60° C. and stirred for an hour. After cooling to room temperature, to the mixture was added water and the product was extracted with ethyl acetate (×3). The combined organic extract was washed successively with water (×1) and brine (×1), followed by drying over anhydrous sodium sulfate. After filtration and concentration under reduced pressure, the residue was purified by silica gel flash column chromatography (n-hexane/ethyl acetate=3/1) to give

1. customat room temperature
2. temperatureAfter cooling to room temperature, to the mixture
3. extractionthe product was extracted with ethyl acetate (×3)
4. extractionThe combined organic extract
5. washwas washed successively with water (×1) and brine (×1)
6. dry with materialby drying over anhydrous sodium sulfate
7. filtrationAfter filtration and concentration under reduced pressure
8. customthe residue was purified by silica gel flash column chromatography (n-hexane/ethyl acetate=3/1)
9. customto give