تفاعل #77841

ord-35c5df770b194cc5a9ffc293550b73f2

معادلة التفاعل

NCCCCCCN
Hexamethylenediamine
CC(N)=O
acetamide
CC(=O)NCCCCCCN
title product
CC(=O)NCCCCCCN
N-acetylhexylendiamine

المتفاعلات

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06706855B1uspto-grants-2004_03