反应详情

In a dry reaction bottle, 16 g (R)-1-[2-formyloxy-5-nitro-6-chloropyridin-4-yl]piperidine-3-carbamic acid tert-butyl ester (40 mmol) was added and dissolved in 50 mL ethanol. 31 g 40% methylamine aqueous solution (400 mmol) was added. The stirring was continued for 2 days at 60° C. The reaction solution was extracted with dichloromethane, dried, and evaporated to dryness to afford a crude product as yellow solid, which was purified through a column chromatography (ethyl acetate:petroleum ether=1:1) to afford 12 g titled product with a yield of 75.9%.

1. additionwas added
2. extractionThe reaction solution was extracted with dichloromethane
3. customdried
4. customevaporated to dryness
5. customto afford a crude product as yellow solid, which
6. customwas purified through a column chromatography (ethyl acetate:petroleum ether=1:1)