反应详情

To 1.00 g of N-[2-(3,5-dichloropyridin-2-yl)-1-methyl-2-oxoethyl]phthalimide in 10 ml of ethanol, 2.39 g of methoxyamine hydrochloride and 3.40 g of pyridine were added and refluxed with heating for 18 hours with stirring. After completion of the reaction, the reaction mixture was allowed to cool to room temperature, mixed with 30 ml of 1N aqueous hydrochloric acid and extracted with ethyl acetate (40 ml×2). The resulting organic layers were combined, washed with 30 ml of 1N aqueous hydrochloric acid and dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 1:9 to 3:7) as the eluent to obtain 0.81 g of the desired product as a colorless resinous substance.

1. temperaturerefluxed
2. temperaturewith heating for 18 hours
3. customAfter completion of the reaction
4. extractionextracted with ethyl acetate (40 ml×2)
5. washwashed with 30 ml of 1N aqueous hydrochloric acid
6. dry with materialdried over saturated aqueous sodium chloride
7. customanhydrous sodium sulfate, and the solvent was evaporated under reduced pressure
8. customThe resulting residue was purified by silica gel column chromatography