反应详情

Benzyl 4-(hydroxymethyl)piperidine-1-carboxylate (2.14 g, 8.57 mmol) was dissolved in dichloromethane (26 mL), to which pyridine (1.04 mL, 12.9 mmol) and p-nitrophenyl chloroformate (2.07 g, 12.9 mmol) were added, followed by stirring at room temperature for 35 minutes under a nitrogen atmosphere. Subsequently, N-methyltetrahydro-2H-pyran-4-amine hydrochloride (1.30 g, 8.57 mmol) and triethylamine (3.59 mL, 25.7 mmol) were added, followed by further stirring for 4.5 hours. Water was added to the resulting reaction liquid, and the resulting mixture was extracted with dichloromethane. The resulting organic layer was dried over sodium sulfate and the solvent was distilled off under reduced pressure. The residue thus obtained was purified by silica gel column chromatography (hexane:ethyl acetate, 100:0-50:50, V/V) to give the desired title compound (2.22 g, yield 66%).

1. additionwere added
2. stirringby further stirring for 4.5 hours
3. extractionthe resulting mixture was extracted with dichloromethane
4. dry with materialThe resulting organic layer was dried over sodium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. customThe residue thus obtained
7. customwas purified by silica gel column chromatography (hexane:ethyl acetate, 100:0-50:50, V/V)