反应详情

温度

25 °C

With cooling, 0.4 g (0.01 mol) of sodium hydride (60%) are added to a mixture of 2 g (0.0096 mol) of 2-(2-hydroxy-phenyl)-2-methoxyimino-N-methyl-acetamide and 2.3 g (0.0095 mol) of 4-(2-chlorophenoxy)-5,6-difluoropyrimidine in 10 ml of dimethylformamide, and the mixture is stirred at 25° C. for 12 hours. The reaction mixture is poured onto water and extracted with dichloromethane, the organic phase is dried over sodium sulphate and the solvent is distilled off under reduced pressure. The residue is chromatographed over silica gel using a mixture of identical volumina of ethyl acetate and cyclohexane. 2.1 g (48.3% of theory) of 2-{2-[6-(2-chlorophenoxy)-5-fluoro-pyrimidine-4-yloxy]-phenyl}-2-methoxyimino-N-methylacetamide are obtained.

1. temperatureWith cooling
2. additionThe reaction mixture is poured onto water
3. extractionextracted with dichloromethane
4. dry with materialthe organic phase is dried over sodium sulphate
5. distillationthe solvent is distilled off under reduced pressure
6. customThe residue is chromatographed over silica gel using
7. additiona mixture of identical volumina of ethyl acetate and cyclohexane