반응 #72100

반응 방정식

potassium carbonate

Carbobenzoxy chloride

diisopropylethylamine

tert-butyl 4-aminopiperidine-1-carboxylate

→

title compound

수율 74.8%

tert-Butyl 4-benzyloxycarbonylaminopiperidine-1-carboxylate

수율 74.8%

용매

ethyl acetate

dichloromethane

반응 조건

후처리

1. 1
   세척washed with brine
2. 2
   건조dried over magnesium sulfate
3. 3
   기타Thereafter, the solvent was evaporated under reduced pressure
4. 4
   기타The resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=3/1)

실험 절차

A solution of tert-butyl 4-aminopiperidine-1-carboxylate (1.2 g, 6 mmol) in dichloromethane (20 mL) was cooled to 0° C. Carbobenzoxy chloride (1.03 mL, 7.2 mmol) and diisopropylethylamine (3.15 mL, 18 mmol) were added at the same temperature, and the solution was stirred at 0° C. for one hour. The reaction solution was neutralized with saturated aqueous potassium carbonate solution, diluted with ethyl acetate, washed with brine, and dried over magnesium sulfate. Thereafter, the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=3/1) to obtain 1.5 g of the title compound as a yellow oily substance (75%).

출처