HRID861900

反应详情

EQUATION

反应方程式

HRID 861900 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of dibromohexane (81.0 g), ethanol (120 ml) and water (50 ml) is added dropwise an aqueous solution (50 ml) of sodium sulfite (12.5 g) under reflux over 2 hours. After additional refluxing for 2 hours, the reaction mixture is allowed to cool and unreacted dibromohexane is removed and then the resulting solution is concentrated under reduced pressure. 95% Ethanol (200 ml) is added and the mixture is allowed to cool at room temperature overnight and precipitated crystals are collected by filtration to give the title compound as colorless prisms. The filtrate is concentrated and is allowed to cool overnight and precipitated crystals are collected by filtration to give additional title compound.

WORKUP

后处理

  1. temperatureunder reflux over 2 hours
  2. temperatureAfter additional refluxing for 2 hours
  3. temperatureto cool
  4. customunreacted dibromohexane is removed
  5. concentrationthe resulting solution is concentrated under reduced pressure
  6. addition95% Ethanol (200 ml) is added
  7. customprecipitated crystals
  8. filtrationare collected by filtration