反应详情

A solution of 3-bromo-6-oxo-1,6-dihydropyridine-2-carbonitrile (from Example 15/Step 2) (1.0 eq.), potassium carbonate (1.3 eq.), and 1-iodobutane (1.2 eq.) in acetone (0.3 M) was stirred at 70° C. overnight. The solvent was concentrated en vacuo, and the resulting residue was taken up in water and ethyl acetate. The aqueous layer was extracted with ethyl acetate three times. The combined organic layers were washed with brine, dried over anhydrous MgSO4, and concentrated en vacuo. The crude product was purified by a COMBIFLASH® system (ISCO) using 0-30% ethyl acetate in hexane to give a colorless solid.

1. customwas stirred at 70° C. overnight
2. concentrationThe solvent was concentrated en vacuo
3. extractionThe aqueous layer was extracted with ethyl acetate three times
4. washThe combined organic layers were washed with brine
5. dry with materialdried over anhydrous MgSO4
6. concentrationconcentrated en vacuo
7. customThe crude product was purified by a COMBIFLASH® system (ISCO)
8. customto give a colorless solid