反应详情

To a mixture of methyl 2-(2-chlorophenyl)-3-(dimethylamino)acrylate 6b (0.26 g, 1.08 mmol), urea (0.2 g, 3.26 mmol) and NaI (0.49 g, 3.26 mmol) in acetonitrile (5 mL) was added TMSCl (0.41 mL, 3.26 mmol). The resulting mixture was refluxed for 16 hours, cooled to room temperature, and 1.0 M NaOH (8 mL) was added. The resultant solution was stirred for 20 hr, and acetonitrile was removed in vacuo. The aq. solution was washed with ether, cooled in ice bath, and neutralized with 1 N HCl (8 mL). The precipitate was filtered, washed with additional H2O, and dried to give 5-(2-chlorophenyl)pyrimidine-2,4(1H,3H)-dione 6c (0.16 g, 66% ) as a white solid. MS (CI) m/z 222.9, 224.9 (MH+).

1. temperatureThe resulting mixture was refluxed for 16 hours
2. customacetonitrile was removed in vacuo
3. washThe aq. solution was washed with ether
4. temperaturecooled in ice bath
5. filtrationThe precipitate was filtered
6. washwashed with additional H2O
7. customdried