tert-butyl 4-(azidomethyl)piperidine-1-carboxylate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Tertiary butyl 4-(azidomethyl)piperidine-1-carboxylate (30 g, 124.8 mmol) was dissolved in tetrahydrofuran (300 mL), and triphenylphosphine (39.3 g, 149.8 mmol) was added thereto, followed by stirring under reflux for 2 hours. Water (120 mL) was added thereto, followed by stirring under reflux for another 3 hours and concentration under reduced pressure. The resulting residue was extracted with ethyl acetate and a 1N hydrochloride solution, and the aqueous layer was neutralized with a 2N sodium hydroxide solution, followed by re-extraction with dichloromethane. The resulting organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to afford the title compound (21.16 g, 79%). under reflux for 2 hours by stirring under reflux for another 3 hours concentration under reduced pressure The resulting residue was extracted with ethyl acetate followed by re-extraction with dichloromethane The resulting organic layer was dried over anhydrous magnesium sulfate concentrated under reduced pressure

反応条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Tertiary butyl 4-((methylsulfonyloxy)methyl)piperidine-1-carboxylate (48 g, 163.6 mmol) was dissolved in dimethylformamide (500 mL) and sodium azide (19.15 g, 295 mmol) was added thereto, followed by stirring at 120° C. for 6 hours. After the reaction was completed, the reactants were cooled to room temperature, extracted with ethyl acetate and water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to afford the title compound (35 g, 89%). the reactants were cooled to room temperature extracted with ethyl acetate and water dried over anhydrous magnesium sulfate concentrated under reduced pressure