反応 #564158

反応方程式

2,2-difluoro-4-methyl-1,3-benzodioxole

Azobisisobutyronitrile

N-bromosuccinimide

→

4-Bromomethyl-2,2-difluoro-1,3-benzodioxole

溶媒

methylene chloride

反応条件

後処理

1. 1
   温度The mixture is then heated
2. 2
   温度under reflux
3. 3
   温度After cooling
4. 4
   ろ過the succinimide is filtered off with suction
5. 5
   洗浄rinsed with carbon tetrachloride
6. 6
   workup.DISTILLATIONthe solution is then distilled in order
7. 7
   その他to separate off the carbon tetrachloride
8. 8
   その他are employed without purification

実験手順

76 g of 2,2-difluoro-4-methyl-1,3-benzodioxole and 200 mg of Azobisisobutyronitrile are added to a suspension of 90 g of N-bromosuccinimide in 400 ml of methylene chloride. The mixture is then heated under reflux, with stirring, until all the undissolved material floats to the top. After cooling, the succinimide is filtered off with suction and rinsed with carbon tetrachloride and the solution is then distilled in order to separate off the carbon tetrachloride. 117 g of crude benzyl bromide remain in the residue and are employed without purification.

出典