反应详情

The above 3-chloro-5-(chloromethyl)-4-methoxy-2-methylpyridine (550 mg) was dissolved in 10 ml of methanol, and 10% Pd carbon (50 mg) was then added to the solution. Normal-pressure contact hydrogenation was performed on the mixture under cooling on ice for 3 hours. Thereafter, the catalyst was removed by filtration, and methanol was then distilled away under reduced pressure. The residue was extracted with chloroform. The organic layer was washed with a saturated sodium bicarbonate solution, and it was then dried over anhydrous sodium sulfate. The solvent was distilled away, and the residue was purified by silica gel chromatography (ethyl acetate-hexane), so as to obtain the title compound (365 mg) as an oily substance.

1. temperatureunder cooling on ice for 3 hours
2. customThereafter, the catalyst was removed by filtration, and methanol
3. distillationwas then distilled away under reduced pressure
4. extractionThe residue was extracted with chloroform
5. washThe organic layer was washed with a saturated sodium bicarbonate solution, and it
6. dry with materialwas then dried over anhydrous sodium sulfate
7. distillationThe solvent was distilled away
8. customthe residue was purified by silica gel chromatography (ethyl acetate-hexane)