HRID37546

反应详情

EQUATION

反应方程式

HRID 37546 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

152.0 g (1.0 mol) of o-vanillin and 200 ml of azeotropic hydrobromic acid (47.5% strength) are stirred under reflux in 500 ml of glacial acetic acid for 2.5 hours. The acid mixture is then distilled off and the residue is subjected to fractional vacuum distillation. The redistilled fraction having a boiling point of 120°-125° C./12 mbar is purified by recrystallisation from 1 l of heptane (hexane is also possible and is recovered). 97 g (70% of theory) of 2,3-dihydroxybenzaldehyde of melting point 105°-107° C. are obtained.

WORKUP

后处理

  1. distillationThe acid mixture is then distilled off
  2. distillationthe residue is subjected to fractional vacuum distillation
  3. customis purified by recrystallisation from 1 l of heptane (hexane
  4. customis recovered)