反应详情

To a solution of tert-butyl 4-formylpiperidine-1-carboxylate (1.0 g, 4.7 mmol) in a mixture of water (5 mL) and methanol (10 mL) were added sodium cyanide (345 mg, 7 mmol) and ammonium carbonate (902 mg, 9.4 mmol) and heated at reflux for 6 h. The reaction mixture was cooled, removed most of the solvent. The crude product was extracted with dichloromethane, dried (Na2SO4) and removed solvent. The crude product was dissolved in dichloromethane (5 mL) and treated with trifluoroacetic acid (5 mL) for 2 h. The solvent was removed and dried. MS (ESI) 184 (M+H); Rf=1.83.

1. temperatureheated
2. temperatureat reflux for 6 h
3. temperatureThe reaction mixture was cooled
4. customremoved most of the solvent
5. extractionThe crude product was extracted with dichloromethane
6. dry with materialdried (Na2SO4)
7. customremoved solvent
8. dissolutionThe crude product was dissolved in dichloromethane (5 mL)
9. additiontreated with trifluoroacetic acid (5 mL) for 2 h
10. customThe solvent was removed
11. customdried