HRID73469

反应详情

EQUATION

反应方程式

HRID 73469 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 73.3 g (0.6 mol) p-hydroxybenzaldehyde, 73.2 g (0.3 mol) 1,6-dibromohexane, 39.6 g (0.6 mol) potassium hydroxide and 240 ml dimethylformamide was heated under reflux, accompanied by stirring for 1 h, in a 500 ml three-necked flask with reflux condenser, internal thermometer and magnetic stirrer. After cooling the reaction mixture to room temperature, the obtained crystal slurry was placed in a 2-1 beaker containing 1 l of deionized water. The formed suspension was stirred intensively by means of a mechanical stirrer until the initially increased temperature had returned to room temperature. The crystals present were then filtered off, washed thoroughly with water and the product recrystallized from a mixture of 1200 ml ethanol and 300 ml water. After drying to constant weight in the vacuum drying cupboard at 70-80° C. 63.5 g (65% of the theoretical value) 1,6-bis(4-formylphenoxy)hexane (m.p.: 109.8-111.2° C.) was obtained in the form of white crystals.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux
  3. temperaturewith reflux condenser
  4. stirringThe formed suspension was stirred intensively by means of a mechanical stirrer until the initially increased temperature
  5. customhad returned to room temperature
  6. filtrationThe crystals present were then filtered off
  7. washwashed thoroughly with water
  8. customthe product recrystallized from a mixture of 1200 ml ethanol and 300 ml water
  9. customAfter drying to constant weight in the vacuum
  10. customdrying cupboard at 70-80° C