HRID1198981

反应详情

EQUATION

反应方程式

HRID 1198981 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 11.7 g (0.05 g mole) of 5-methyl-3-phenyl-2,1-benzisoxazole, 10.0 g (0.056 mole) of N-bromosuccinimide and 0.1 g of dibenzoylperoxide in 200 ml of carbon tetrachloride was heated at reflux under illumination by a flood lamp for 2.5 hr. The mixture was filtered and the filtrate was washed with 5% sodium hydroxide, dried over sodium sulfate and concentrated to give a solid as residue. This solid was recrystallized twice from 2-propanol to yield 9.5 g (59%) of crystals, m.p. 130° C. (with decomposition).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux under illumination by a flood lamp for 2.5 hr
  3. filtrationThe mixture was filtered
  4. washthe filtrate was washed with 5% sodium hydroxide
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customto give a solid as residue
  8. customThis solid was recrystallized twice from 2-propanol