Triethylamine → HCID 70975548, compound

Participants

Reaction Conditions

Reaction Steps

1.42 g triphosgene (4.78 mmol) was dissolved in 10 mL dichloromethane, and cooled to −10° C. 1.77 mL triethylamine (12.72 mmol) was added. A solution of 1.5 g (R)-1-[2-(2,4-dimethoxybenzyl)amino-6-methyl-3-aminopyridin-4-yl]piperidine-3-carbamic acid tert-butyl ester (3.18 mmol) in dichloromethane (20 mL) was slowly added dropwise at −10° C. After they were completely reacted, the reaction solution was adjusted to be basic by adding saturated sodium carbonate solution, and extracted twice with dichloromethane. The combined organic phase was washed with brine, dried with anhydrous sodium sulfate, and evaporated to dryness. The resultant crude product was recrystallized with dichloromethane and ethyl acetate to afford 1.03 g titled product with a yield of 65.2%.

Provenance & Evidence