反应详情

To 50 ml of a butanol solution of 9.376 g of 2-chloro-3-methoxypyridine were added 16 ml of hydrazine monohydrate and 9.03 g of anhydrous potassium carbonate, and the mixture was heated under reflux for 20 hours. After cooling, the reaction mixture was poured into 200 ml of water and extracted with a mixed solvent of methanol-chloroform (1:9 by volume). The organic layer was washed with a saturated sodium chloride aqueous solution, and dried over anhydrous sodium sulfate. The solvent was removed by evaporation. The residue was subjected to silica gel column chromatography using a mixture of chloroform-methanol (20:1 by volume) as an eluate. The fraction containing the desired compound was concentrated to afford 5.952 g of the title compound.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 20 hours
3. temperatureAfter cooling
4. extractionextracted with a mixed solvent of methanol-chloroform (1:9 by volume)
5. washThe organic layer was washed with a saturated sodium chloride aqueous solution
6. dry with materialdried over anhydrous sodium sulfate
7. customThe solvent was removed by evaporation
8. additiona mixture of chloroform-methanol (20:1 by volume) as an eluate
9. additionThe fraction containing the desired compound
10. concentrationwas concentrated