HRID1438811

反应详情

EQUATION

反应方程式

HRID 1438811 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of pyrogallol (63 parts) in 2,2-dimethoxypropane (100 parts) and benzene (100 parts) containing toluenesulphonic acid (0.01 parts) was slowly distilled through a fractionating column during 4 hours, removing liquid (150 parts), boiling point 57°-64° C. A few drops of triethylamine were then added and the mixture thoroughly washed with water, dried and evaporated. Distillation gave 4-hydroxy-2,2-dimethyl-1,3-benzodioxole (36 parts), boiling point 110° C/0.7 mm., which was purified by recrystallisation from carbon tetrachloride. Melting point 88°-90° C.

WORKUP

后处理

  1. distillationwas slowly distilled through a fractionating column during 4 hours
  2. customremoving liquid (150 parts), boiling point 57°-64° C
  3. additionA few drops of triethylamine were then added
  4. washthe mixture thoroughly washed with water
  5. customdried
  6. customevaporated
  7. distillationDistillation