تفاعل #43897

ord-5d449bcf8e7f4469af6a74da47b5a3ab

معادلة التفاعل

CC1=CCC(CC=O)C1(C)C
campholenic aldehyde
CCC=O
propionaldehyde
CC(C=O)=CCC1CC=C(C)C1(C)C
2-methyl-4-(2,2,3-trimethylcyclopent-3-en-1-yl)-but-2-en-1-al
المردود 94.9%

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىA 500 mL four-necked flask equipped with a stirrer
  2. 2
    درجة الحرارةcooled
  3. 3
    أخرىto remove amines
  4. 4
    أخرىseparating the mixture into two layers
  5. 5
    غسيلThe thus separated organic layer was washed with water
  6. 6
    أخرىseparated into two layers

الإجراء التجريبي

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%), 3.8 g (0.045 mol) of piperidine and 13.1 g (0.046 mol) of stearic 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 separated into two layers, thereby obtaining 295 g (0.93 mol) of 2-methyl-4-(2,2,3-trimethylcyclopent-3-en-1-yl)-but-2-en-1-al (purity as measured by gas chromatography: 60.6%) (yield based on theoretical amount: 95%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07732644B2uspto-grants-2010_06