HRID378498
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
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.
WORKUP
后处理
- temperatureunder reflux for 28 hours until the originally yellow suspension
- distillationAfter distilling off the solvent
- extractionthe reaction mixture is extracted twice with diethyl ether (2×250 ml), and insoluble salts
- filtrationare filtered off
- washThe filtrate is washed twice with 200 ml water
- dry with materialdried over Na2SO4
- distillationThe solvent is then distilled off
- washThe colourless, solid residue is washed twice with petroleum ether
- customrecrystallized from petroleum ether