反应详情

温度

100 °C

30 g of 3-[4-chloro-2,6-difluoro-3-nitrophenyl]-1-methyl-6-trifluoromethyl-2,4-(1H,3H)-pyrimidinedione were dissolved in 100 ml of absolute dimethylformamide, admixed with 25.2 g of sodium acetate and heated at 100° C. for four hours. After cooling, the solvent was removed under reduced pressure and the residue was admixed with water; by addition of dilute hydrochloric acid, the pH was taken into the acidic range, and the mixture was extracted with methyl tert-butyl ether (three times 75 ml). The product of value was obtained as a mixture with the isomer formed by exchange of the fluorine atom which is in the position para to the nitro group. Total yield: 28.3 g. The crude product was purified at the subsequent stage (intermediate 7).

1. temperatureAfter cooling
2. customthe solvent was removed under reduced pressure
3. additionby addition of dilute hydrochloric acid
4. extractionthe mixture was extracted with methyl tert-butyl ether (three times 75 ml)
5. customThe product of value was obtained as a mixture with the isomer
6. customformed by exchange of the fluorine atom which
7. customThe crude product was purified at the subsequent stage (intermediate 7)