반응 #43901

반응 방정식

hydroxycitronellal

formaldehyde

dibutyl amine

hexanoic acid

hydroxycitronellal

→

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

반응 조건

후처리

1. 1
   기타A 3 L four-necked flask equipped with a stirrer
2. 2
   기타After the elapse of 40 min, it
3. 3
   온도the mixture was cooled
4. 4
   기타separated into two layers
5. 5
   workup.DISTILLATIONThe thus separated organic layer was subjected to distillation treatment

실험 절차

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%).

출처