反应详情

In a dry reaction bottle, 8.32 g triphosgene (28 mmol) and 7.8 mL triethylamine (56 mmol) were added and dissolved in 240 mL tetrahydrofuran. A solution of 5.31 g (R)-1-[2-methoxycarbonyl-5-amino-6-methylaminopyridin-4-yl]piperidine-3-carbamic acid tert-butyl ester (14 mmol) in tetrahydrofuran (80 mL) was added dropwise at −10° C. After addition, the reaction solution was adjusted to be neutral with saturated sodium carbonate solution. Water and dichloromethane were added to the reaction solution. The reaction solution was extracted with dichloromethane. The organic phase was combined, washed with saturated brine, dried with anhydrous sodium sulfate, evaporated to remove dichloromethane, washed with ethyl acetate, filtrated, and dried to afford 4.1 g titled product as white solid, with a yield of 72.3%.

1. additionwere added
2. additionAfter addition
3. extractionThe reaction solution was extracted with dichloromethane
4. washwashed with saturated brine
5. dry with materialdried with anhydrous sodium sulfate
6. customevaporated
7. customto remove dichloromethane
8. washwashed with ethyl acetate
9. filtrationfiltrated
10. customdried