反应详情

温度

0 °C

To 7.0 g of 3 hydroxypicolinic acid, 10 ml of N,N-dimethylformamide was added, and then 5.9 g of thionyl chloride was dropwise added thereto at a temperature of at most 10° C. The mixture was stirred at 0° C. for 30 minutes. To the reaction solution, 30 ml of chloroform was added, and the mixture was further stirred at 0° C. for 15 minutes. Then, a solution prepared by dissolving 5.0 g of diethyl ketone oxime in 50 ml of chloroform was dropwise added thereto at 0° C., and the mixture was stirred for 30 minutes. Then, 7.9 g of pyridine was dropwise added thereto. Then, the reaction solution was stirred at 0° C. for one hour and at room temperature for one day. The reaction solution was poured into water and extracted with ethyl acetate. Then, the extract was washed with a saturated sodium hydrogencarbonate aqueous solution and with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue thereby obtained was purified by silica gel column chromatography by using as a developing solvent a mixture of hexane/ethyl ether to obtain 6.5 g of the above identified compound as slightly yellow transparent viscous liquid.

1. customat a temperature of at most 10° C
2. stirringthe mixture was further stirred at 0° C. for 15 minutes
3. customThen, a solution prepared
4. additionwas dropwise added
5. stirringat 0° C., and the mixture was stirred for 30 minutes
6. stirringThen, the reaction solution was stirred at 0° C. for one hour and at room temperature for one day
7. extractionextracted with ethyl acetate
8. washThen, the extract was washed with a saturated sodium hydrogencarbonate aqueous solution and with a saturated sodium chloride aqueous solution
9. dry with materialdried over anhydrous sodium sulfate
10. distillationThe solvent was distilled off under reduced pressure
11. customthe residue thereby obtained
12. customwas purified by silica gel column chromatography
13. additiona mixture of hexane/ethyl ether
14. customto obtain 6.5 g of the