반응 #75874

반응 방정식

Ethyl 4-amino-1-piperidinecarboxylate

triethylamine

t-butylsulfinyl chloride

→

amino-1-ethoxycarbonyl piperidine

수율 126.0%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   기타The solution was partitioned into an aqueous solution of potassium hydrogen sulfate and ethyl acetate
2. 2
   세척The organic layer was washed with brine
3. 3
   건조dried over magnesium sulfate anhydride
4. 4
   기타The solvent was removed under reduced pressure
5. 5
   기타the residue was purified by silica gel chromatography

실험 절차

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.

출처