Реакция #1483047

Уравнение реакции

N,N-dibutylamine

Valeroyl chloride

dibutylamine

→

N,N-dibutylpentanamide

Растворители

diethyl ether

diethyl ether

Условия реакции

Обработка

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

Методика

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.

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