反应详情

温度

80 °C

To a solution of 4-aminocarbonyl-1-(1-naphthylsulfonyl)piperidine (10.6 g, 33.3 mmol) in tetrahydrofuran (200 mL) stirring under argon at room temperature, was added borane-tetrahydrofuran complex (1.5 M in tetrahydrofuran, 67 mL, 100 mmol). The resulting solution was heated to 80° C. for 6 h before the solvent was evaporated under vacuum. The residue was dissolved in 1.0 M aqueous hydrochloric acid (100 mL), and this was washed with diethyl ether (100 mL twice). The aqueous layer was basified to pH 10 with 50% aqueous sodium hydroxide and extracted with dichloromethane (50 mL three times). The combined dichloromethane extracts were dried (anhydrous sodium sulfate) and evaporated under vacuum to obtain 4-aminomethyl-1-(1-naphthylsulfonyl)piperidine (9.1 g, 90% yield).

1. customwas evaporated under vacuum
2. dissolutionThe residue was dissolved in 1.0 M aqueous hydrochloric acid (100 mL)
3. washthis was washed with diethyl ether (100 mL twice)
4. extractionextracted with dichloromethane (50 mL three times)
5. dry with materialThe combined dichloromethane extracts were dried (anhydrous sodium sulfate)
6. customevaporated under vacuum