反応 #43899

ord-ed318f7105764e938d27aaa8efcdf566

反応方程式

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

反応条件

温度
95°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07732644B2uspto-grants-2010_06