反応 #43900

反応方程式

n-octanal

formaldehyde

dibutyl amine

decanoic acid

n-octanal

→

a-methylene octanal

反応条件

後処理

1. 1
   その他A 2 L four-necked flask equipped with a stirrer
2. 2
   その他After the elapse of 45 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 2 L four-necked flask equipped with a stirrer, a thermometer and a reflux condenser was charged with 762 g (6.0 mol) of n-octanal, 520 g (6.4 mol) of a 37% by mass formaldehyde aqueous solution, 15 g (0.33 mol) of dibutyl amine and 10 g (0.06 mol) of decanoic acid, and the contents in the flask were stirred while heating at 95° C. After the elapse of 45 min, it was confirmed that no n-octanal 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 790 g (5.4 mol) of a-methylene octanal (purity as measured by gas chromatography: 95%) (yield based on theoretical amount: 90%).

出典