Azobisisobutyronitrile → 4-(Bromomethyl)-2,2-difluoro-1,3-dioxaindane
反応式
[F:1][C:2]1([F:12])[O:6][C:5]2[CH:7]=[CH:8][CH:9]=[C:10]([CH3:11])[C:4]=2[O:3]1.N(C(C)(C)C#N)=NC(C)(C)C#N.[Br:25]N1C(=O)CCC1=O>C(Cl)Cl>[Br:25][CH2:11][C:10]1[C:4]2[O:3][C:2]([F:1])([F:12])[O:6][C:5]=2[CH:7]=[CH:8][CH:9]=1参加物
5
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.
後処理
- temperatureThe mixture is then heated
- temperatureunder reflux
- temperatureAfter cooling
- filtrationthe succinimide is filtered off with suction
- washrinsed with carbon tetrachloride
- distillationthe solution is then distilled in order
- customto separate off the carbon tetrachloride
- customare employed without purification
出典と根拠
- ORDレコード
- ord-75599d6ab0d0407dba57eb512a4a4053
- 出典データセット
- uspto-grants-1989_12
- 特許番号
- US04886816
反応ノート
読み込み中…