反应详情

温度

80 °C

50% Aqueous hydroxylamine solution (40 g) was added to a methanol (100 mL) and tetrahydrofuran (100 mL) solution containing methyl 3-[4-(5-cyanopyridin-2-yl)-phenoxy]-2,2-dimethylpropanoate (6.0 g), and the mixture was stirred at 80° C. for 4 hours. After cooling the reaction mixture to room temperature, the mixture was concentrated under reduced pressure. To the obtained residue were added ethyl acetate and water, and the liquids were separated. The organic layer was separated, washed with water, and dried over anhydrous sodium sulfate. Ether was added to the solid residue obtained by concentrating the mixture under reduced pressure to pulverize the same, and the solid was collected by filtration and dried to obtain methyl 3-(4-{5-[amino(hydroxyimino)methyl]pyridin-2-yl}phenoxy)-2,2-dimethylpropanoate (5.8 g).

1. temperatureAfter cooling the reaction mixture to room temperature
2. concentrationthe mixture was concentrated under reduced pressure
3. additionTo the obtained residue were added ethyl acetate and water
4. customthe liquids were separated
5. customThe organic layer was separated
6. washwashed with water
7. dry with materialdried over anhydrous sodium sulfate
8. additionEther was added to the solid residue
9. customobtained
10. concentrationby concentrating the mixture under reduced pressure
11. filtrationwas collected by filtration
12. customdried