HRID1198981
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureat reflux under illumination by a flood lamp for 2.5 hr
- filtrationThe mixture was filtered
- washthe filtrate was washed with 5% sodium hydroxide
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- customto give a solid as residue
- customThis solid was recrystallized twice from 2-propanol