تفاعل #465680

معادلة التفاعل

diethyl-2,5-dihydroxyterephthalate

1,10-dibromodecane

K2CO3

NaI

→

diethyl-2,5-bis-(10-bromodecoxy)terephthalate

المذيبات

acetone

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةunder reflux for 28 hours until the originally yellow suspension
2. 2
   workup.DISTILLATIONAfter distilling off the solvent
3. 3
   استخلاصthe reaction mixture is extracted twice with diethyl ether (2×250 ml), and insoluble salts
4. 4
   ترشيحare filtered off
5. 5
   غسيلThe filtrate is washed twice with 200 ml water
6. 6
   تجفيفdried over Na2SO4
7. 7
   workup.DISTILLATIONThe solvent is then distilled off
8. 8
   غسيلThe colourless, solid residue is washed twice with petroleum ether
9. 9
   أخرىrecrystallized from petroleum ether

الإجراء التجريبي

25.4 g (0.1 mol) diethyl-2,5-dihydroxyterephthalate, 450 g (1.5 mol) 1,10-dibromodecane, 138 g (1.0 mol) K2CO3 and 200 mg NaI in 200 ml acetone are heated under reflux for 28 hours until the originally yellow suspension has decolorized. After distilling off the solvent, the reaction mixture is extracted twice with diethyl ether (2×250 ml), and insoluble salts are filtered off. The filtrate is washed twice with 200 ml water and dried over Na2SO4. The solvent is then distilled off. The colourless, solid residue is washed twice with petroleum ether and then recrystallized from petroleum ether.

المصدر