HRID1902814

反应详情

EQUATION

反应方程式

HRID 1902814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Eighty grams of the crude 1,2,4-triacetoxybenzene were dissolved in 200 ml of methanol containing 6 g of concentrated sulfuric acid. The reaction mixture was boiled under reflux for one hour. Then the solution was cooled to room temperature and neutralized with an equivalent amount of fine powdered sodium carbonate. Thereafter 800 ml of ethylether was added whereupon sodium sulfate precipitated out, which was removed by filtration. Reaction by-products and contaminants being responsible for a dark red coloration may be removed employing solid silica gel. After evaporation of the supernatant under reduced pressure, a dark red oil is obtained which crystallized upon standing at 40° C. in the form of a slight reddish solid mass which is pure enough for the next step. This product is 1,2,4-trihydroxybenzene.

WORKUP

后处理

  1. temperatureunder reflux for one hour
  2. customprecipitated out
  3. customwhich was removed by filtration
  4. customReaction by-products and contaminants
  5. custommay be removed
  6. customAfter evaporation of the supernatant under reduced pressure
  7. customa dark red oil is obtained which
  8. customcrystallized
  9. customupon standing at 40° C. in the form of a slight reddish solid mass which