反应 #75874

反应方程式

Ethyl 4-amino-1-piperidinecarboxylate

triethylamine

t-butylsulfinyl chloride

→

amino-1-ethoxycarbonyl piperidine

收率 126.0%

溶剂

dichloromethane

dichloromethane

反应条件

后处理

1. 1
   其他The solution was partitioned into an aqueous solution of potassium hydrogen sulfate and ethyl acetate
2. 2
   洗涤The organic layer was washed with brine
3. 3
   干燥dried over magnesium sulfate anhydride
4. 4
   其他The solvent was removed under reduced pressure
5. 5
   其他the residue was purified by silica gel chromatography

实验过程

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.

来源