HRID1733460

反应详情

EQUATION

反应方程式

HRID 1733460 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

21.5 g (0.12 mol) of freshly distilled 1-bromo-5-hexanone are dissolved in 200 ml of absolute ethanol in a 500 ml capacity flask, followed by the gradual dropwise addition at boiling temperature of 34.7 g (0.12 mol) of sodium 1,3-dibutyl xanthine dissolved in 200 ml of absolute ethanol. The solution is heated under reflux. The reaction is over after about 24 hours. Removal of the alcohol by distillation in a rotary evaporator leaves a solid white residue. This residue is introduced into an extraction tube in which it is extracted with petrol 40/80 in a Soxhlet apparatus until no more starting material can be detected. The petrol is distilled off in a rotary evaporator, leaving 25 g (0.069 mol) of 7-(5'-oxohexyl)-1,3-dibutyl xanthine, corresponding to 75% of the theoretical, based on the sodium 1,3-dibutyl xanthine reacted.

WORKUP

后处理

  1. temperatureThe solution is heated
  2. temperatureunder reflux
  3. customafter about 24 hours
  4. customRemoval of the alcohol
  5. distillationby distillation
  6. customin a rotary evaporator
  7. customleaves a solid white residue
  8. additionThis residue is introduced into an extraction tube in which it
  9. extractionis extracted with petrol 40/80 in a Soxhlet apparatus until
  10. distillationThe petrol is distilled off in a rotary evaporator