Reaktion #75874
ord-61139bc34ed540e5864fa7318d8e13b7
Reaktionsgleichung
Ethyl 4-amino-1-piperidinecarboxylate
triethylamine
t-butylsulfinyl chloride
→
amino-1-ethoxycarbonyl piperidine
Ausbeute 126.0%
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeThe solution was partitioned into an aqueous solution of potassium hydrogen sulfate and ethyl acetate
- 2WaschenThe organic layer was washed with brine
- 3Trocknendried over magnesium sulfate anhydride
- 4SonstigeThe solvent was removed under reduced pressure
- 5Sonstigethe residue was purified by silica gel chromatography
Vorschrift
Ethyl 4-amino-1-piperidinecarboxylate (300 mg) and triethylamine (258 mg) were dissolved in 5 ml of dichloromethane. To the mixture, 2 ml of solution of t-butylsulfinyl chloride (222 mg) in dichloromethane was added and the mixture was stirred at room temperature for 4 hours. The solution was partitioned into an aqueous solution of potassium hydrogen sulfate and ethyl acetate. The organic layer was washed with brine and dried over magnesium sulfate anhydride. The solvent was removed under reduced pressure and the residue was purified by silica gel chromatography to give 378 mg of 4-t-butylsulfiny amino-1-ethoxycarbonyl piperidine.