Reaktion #43899

ord-ed318f7105764e938d27aaa8efcdf566

Reaktionsgleichung

CCCCCCCCCCC=O
n-undecanal
C=O
formaldehyde
CCCCNCCCC
dibutyl amine
CCCCCCCCCCCCCCCCCC(=O)O
stearic acid
CCCCCCCCCCC=O
n-undecanal
C=C(C=O)CCCCCCCCC
α-methylene undecanal

Reaktionsbedingungen

Temperatur
95°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA 3 L four-necked flask equipped with a stirrer
  2. 2
    SonstigeAfter the elapse of 30 min. it
  3. 3
    Temperaturthe mixture was cooled
  4. 4
    Sonstigeseparated into two layers
  5. 5
    workup.DISTILLATIONThe thus separated organic layer was subjected to distillation treatment

Vorschrift

A 3 L four-necked flask equipped with a stirrer, a thermometer and a reflux condenser was charged with 1043 g (6.0 mol) of n-undecanal, 520 g (6.4 mol) of a 37% by mass formaldehyde aqueous solution, 47 g (0.36 mol) of dibutyl amine and 33 g (0.11 mol) of stearic acid, and the contents in the flask were stirred while heating at 95° C. After the elapse of 30 min. it was confirmed that no n-undecanal was present in the raw mixture, and then the mixture was cooled and separated into two layers. The thus separated organic layer was subjected to distillation treatment, thereby obtaining 1062 g (5.7 mol) of α-methylene undecanal (purity as measured by gas chromatography: 97%) (yield based on theoretical amount: 95%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732644B2uspto-grants-2010_06