反応 #43898

反応方程式

campholenic aldehyde

propionaldehyde

→

2-methyl-4-(2,2,3-trimethylcyclopent-3-en-1-yl)-but-2-en-1-al

収率 93.9%

反応条件

後処理

1. 1
   その他A 500 mL four-necked flask equipped with a stirrer
2. 2
   温度cooled
3. 3
   その他to remove amines
4. 4
   その他separating the mixture into two layers
5. 5
   洗浄The thus separated organic layer was washed with water
6. 6
   その他further separated into two layers

実験手順

A 500 mL four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a dropping funnel was charged with 171 g (0.98 mol) of campholenic aldehyde (purity: 88%), 5.8 g (0.045 mol) of dibutyl amine and 5.3 g (0.046 mol) of hexanoic acid, and the contents in the flask were stirred while heating at 100° C. Then, 91 g (1.6 mol) of propionaldehyde was gradually dropped into the flask for 6 h, and the resultant mixture was aged for 1 h and then cooled. Thereafter, 3.2 g (0.053 mol) of acetic acid was added to the mixture to remove amines therefrom, thereby separating the mixture into two layers. The thus separated organic layer was washed with water and further separated into two layers, thereby obtaining 280 g (0.92 mol) of 2-methyl-4-(2,2,3-trimethylcyclopent-3-en-1-yl)-but-2-en-1-al (purity as measured by gas chromatography: 63.4%) (yield based on theoretical amount: 94%).

出典