HRID378495

反应详情

EQUATION

反应方程式

HRID 378495 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

25.4 g (0.1 mol) diethyl-2,5-dihydroxyterephthalate, 232 ml (1.5 mol) 1,6-dibromohexane, 130 g (0.94 mol) K2CO3 and 200 mg NaI in 200 ml acetone are heated under reflux for 12 hours. The initially yellow suspension decolorizes. After distilling off the solvent, 1200 ml diethyl ether are added to the reaction mixture and the whole is washed twice, each time with 200 ml water. The organic phase is then dried over Na2SO4 and the solvent is distilled off. The colourless product which crystallized out after adding 250 ml petroleum ether at -20° C. is recrystallized once from petroleum ether and twice from ethanol.

WORKUP

后处理

  1. temperatureunder reflux for 12 hours
  2. distillationAfter distilling off the solvent, 1200 ml diethyl ether
  3. additionare added to the reaction mixture
  4. washthe whole is washed twice
  5. dry with materialThe organic phase is then dried over Na2SO4
  6. distillationthe solvent is distilled off
  7. customThe colourless product which crystallized out
  8. additionafter adding 250 ml petroleum ether at -20° C.
  9. customis recrystallized once from petroleum ether and twice from ethanol