反応 #1483047

反応方程式

N,N-dibutylamine

Valeroyl chloride

dibutylamine

→

N,N-dibutylpentanamide

溶媒

diethyl ether

diethyl ether

反応条件

後処理

1. 1
   workup.ADDITIONa round-bottom flask containing a magnetic stirring bar
2. 2
   その他The flask was removed from ice
3. 3
   抽出Two 500 mL extractions
4. 4
   その他to remove the excess amine and ammonium chloride byproduct
5. 5
   乾燥dried with MgSO4
6. 6
   その他Diethyl ether was removed under rotary evaporation and high vacuum

実験手順

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.

出典