反应详情

Chloroactonitrile (16.5 g) and potassium carbonate (29.3 g) were added to a solution of 6-chloro-3-propylpyrimidine-2,4(1H,3H)-dione (20 g) in DMF (200 ml), and the mixture was stirred at room temperature for 24 hours. The reaction solution was concentrated and evaporated to dryness to obtain a residue. A resulting residue was dissolved in chloroform and H2O, and the organic layer was washed with water and dried. The solvent was evaporated to dryness to give a syrup, which was purified by column chromatography on silica gel to give a crystalline product. Recrystalization of the crude crystals from ethyl acetate-isopropylether gave colorless prisims (21.1 g, 87%), mp. 83°-84° C.

1. concentrationThe reaction solution was concentrated
2. customevaporated to dryness
3. customto obtain a residue
4. washH2O, and the organic layer was washed with water
5. customdried
6. customThe solvent was evaporated to dryness
7. customto give a syrup, which
8. customwas purified by column chromatography on silica gel
9. customto give a crystalline product
10. customRecrystalization of the crude crystals from ethyl acetate-isopropylether
11. customgave colorless prisims (21.1 g, 87%), mp. 83°-84° C.