HRID2080803

反应详情

EQUATION

反应方程式

HRID 2080803 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The mixture (4.02 g) obtained in Example 36-1 in a carbon tetrachloride solution (45 ml) was added with N-bromosuccinimide (1.31 g) and 2,2′-azobisisobutyronitrile (0.121 g) and the whole was refluxed for 30 minutes. After that, the solution was cooled to room temperature and a solid component was separated by filtration. The organic layer was washed with a 1 mol/l sodium hydroxide aqueous solution and a saturated saline solution in the stated order, and dried with anhydrous magnesium sulfate. The solvent was distilled off and dried under reduced pressure, thereby obtaining a mixture (5.72 g) containing the subject compound.

WORKUP

后处理

  1. temperaturethe whole was refluxed for 30 minutes
  2. customa solid component was separated by filtration
  3. washThe organic layer was washed with a 1 mol/l sodium hydroxide aqueous solution
  4. dry with materiala saturated saline solution in the stated order, and dried with anhydrous magnesium sulfate
  5. distillationThe solvent was distilled off
  6. customdried under reduced pressure