反応 #77841

反応方程式

Hexamethylenediamine

acetamide

→

title product

N-acetylhexylendiamine

反応条件

後処理

1. 1
   温度refluxed for 10 hours under nitrogen
2. 2
   温度The solution was cooled overnight
3. 3
   workup.DISTILLATIONdistilled under vacuum <100° C. as fast as possible
4. 4
   その他The N-acetylhexylenediamine was then separated from the resultant mixture by flash chromatography [SiO2/EtOH:25%aq.NH3 (4:1)]

実験手順

Hexamethylenediamine (90.64 g; 0.6 mol) and acetamide (11.81 g; 0.2 Mol) were stirred and refluxed for 10 hours under nitrogen. The solution was cooled overnight and then distilled under vacuum <100° C. as fast as possible. The N-acetylhexylenediamine was then separated from the resultant mixture by flash chromatography [SiO2/EtOH:25%aq.NH3 (4:1)]. The title product was obtained as a white crystalline product (18.43 g; 58% theory).

出典