HRID704002

反应详情

EQUATION

反应方程式

HRID 704002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5.64 g (29 mM) of 4-n-butylveratrole, 18.54 g (309 mM) of acetic acid and 55.62 g (323 mM) of 47% hydrobromic acid was heated under reflux for 4 hours with stirring. The reaction mixture wa cooled to the room temperature and added with 50 ml of water. The separated oil was extracted with ether. The ether solution was successively washed with 50 ml of water, 75 g of 5% aqueous sodium thiosulfate solution, and further twice with each 50 ml of water. The resulting solution was dried with anhydrous sodium sulfate, distilled off ether, and vacuum distilled to obtain 3.89 g (23 mM) of 4-n-butylcatechol as light yellow liquid having a boiling point of 125° C./3 mmHg.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 4 hours
  3. extractionThe separated oil was extracted with ether
  4. washThe ether solution was successively washed with 50 ml of water, 75 g of 5% aqueous sodium thiosulfate solution
  5. dry with materialThe resulting solution was dried with anhydrous sodium sulfate
  6. distillationdistilled off ether, and vacuum
  7. distillationdistilled