반응 #1483047

반응 방정식

N,N-dibutylamine

Valeroyl chloride

dibutylamine

→

N,N-dibutylpentanamide

용매

diethyl ether

diethyl ether

반응 조건

후처리

1. 1
   workup.ADDITIONa round-bottom flask containing a magnetic stirring bar
2. 2
   기타The flask was removed from ice
3. 3
   추출Two 500 mL extractions
4. 4
   기타to remove the excess amine and ammonium chloride byproduct
5. 5
   건조dried with MgSO4
6. 6
   기타Diethyl ether was removed under rotary evaporation and high vacuum

실험 절차

a round-bottom flask containing a magnetic stirring bar, diethyl ether (400 mL) and N,N-dibutylamine (37 mL, 0.22 mol, 2.2 equiv.) was cooled in ice for 30 minutes. Valeroyl chloride (12.0 mL, 0.099 mol, 1.0 equiv.) was combined with diethyl ether (75 mL) and added dropwise over 30 minutes to the stirring dibutylamine solution on ice. A white precipitate, likely the amine's chloride salt, was observed. The flask was removed from ice and stirred at room temperature for 3 h. Two 500 mL extractions were performed with dilute HCl (10 mL conc. HCl per 500 mL extraction) to remove the excess amine and ammonium chloride byproduct. The diethyl ether layer was retained and dried with MgSO4. Diethyl ether was removed under rotary evaporation and high vacuum, leaving crude N,N-dibutylpentanamide.

출처