Reaktion #43901

Reaktionsgleichung

hydroxycitronellal

formaldehyde

dibutyl amine

hexanoic acid

hydroxycitronellal

→

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

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeA 3 L four-necked flask equipped with a stirrer
2. 2
   SonstigeAfter the elapse of 40 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 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%).

Quelle