反応 #43901

反応方程式

hydroxycitronellal

formaldehyde

dibutyl amine

hexanoic acid

hydroxycitronellal

→

3,7-dimethyl-2-methylene-7-hydroxyoctanal

反応条件

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 40 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 1032 g (6.0 mol) of hydroxycitronellal, 520 g (6.4 mol) of a 37% by mass formaldehyde aqueous solution, 53 g (0.41 mol) of dibutyl amine and 10 g (0.09 mol) of hexanoic acid, and the contents in the flask were stirred while heating at 95° C. After the elapse of 40 min, it was confirmed that no hydroxycitronellal 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 1058 g (5.5 mol) of 3,7-dimethyl-2-methylene-7-hydroxyoctanal (purity as measured by gas chromatography: 95%) (yield based on theoretical amount: 92%).

出典