Azobisisobutyronitrile → 4-(Bromomethyl)-2,2-difluoro-1,3-dioxaindane
반응식
[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]=1참가 물질
5
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-75599d6ab0d0407dba57eb512a4a4053
- 출처 데이터셋
- uspto-grants-1989_12
- 특허 번호
- US04886816
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