تفاعل #313383

معادلة التفاعل

2-hydroxy-5-hexenoic acid

toluene

p-toluenesulfonic acid

→

3,6-di(3-butenyl)-1,4-dioxane-2,5-dione

المردود 41.0%

المذيبات

Water

ظروف التفاعل

المعالجة

1. 1
   أخرىIn a 1-L flask equipped with a reflux condenser
2. 2
   درجة الحرارةrefluxed under a nitrogen atmosphere
3. 3
   درجة الحرارةThe mixture was cooled
4. 4
   درجة الحرارةafter refluxing for 72 hours
5. 5
   غسيلIt was washed twice with 10 ml of a saturated aqueous solution of sodium hydrogencarbonate
6. 6
   أخرىan obtained crude product
7. 7
   workup.DISTILLATIONdistilled in the presence of zinc oxide

الإجراء التجريبي

In a 1-L flask equipped with a reflux condenser and a Dean-Stark trap, 3.0 g of 2-hydroxy-5-hexenoic acid, 400 ml of toluene and 30 mg of p-toluenesulfonic acid were added and refluxed under a nitrogen atmosphere. Water accumulated in the trap was eliminated from time to time. The mixture was cooled after refluxing for 72 hours. It was washed twice with 10 ml of a saturated aqueous solution of sodium hydrogencarbonate, and an obtained crude product was vacuum distilled in the presence of zinc oxide to obtain 1.06 g of desired 3,6-di(3-butenyl)-1,4-dioxane-2,5-dione (yield 41%).

المصدر