Реакция #43901

Уравнение реакции

hydroxycitronellal

formaldehyde

dibutyl amine

hexanoic acid

hydroxycitronellal

→

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

Условия реакции

Обработка

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

Методика

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%).

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