Azobisisobutyronitrile → HCID 19068194, 화합물
반응식
[CH2:1]([C:3]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[O:5][N:4]=1)[CH3:2].[Br:12]N1C(=O)CCC1=O.CC(N=NC(C#N)(C)C)(C#N)C>C(Cl)(Cl)(Cl)Cl>[Br:12][CH:1]([C:3]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[O:5][N:4]=1)[CH3:2]참가 물질
5
실험 절차
A mixture of 5.3 g of 3-ethyl-1,2-benzisoxazole, 6.4 g of N-bromosuccinimide and 50 ml of carbon tetrachloride is refluxed for 1 h. Afterwards c. 50 mg of α,α-azoisobutyro-nitrile are added and the mixture is refluxed for a further 1 h. After cooling and filtering the mixture, the filtrate is concentrated under vacuum. The crude product is purified by chromatography over silica gel with ethyl acetate/hexane (1:1) to give 3-(1-bromoethyl)-1,2-benzisoxazole as an oil.
후처리
- temperatureis refluxed for 1 h
- temperaturethe mixture is refluxed for a further 1 h
- temperatureAfter cooling
- filtrationfiltering the mixture
- concentrationthe filtrate is concentrated under vacuum
- customThe crude product is purified by chromatography over silica gel with ethyl acetate/hexane (1:1)
출처 및 근거
- ORD 기록
- ord-3ae79d8669ac42dcb952e4e0f37298ea
- 출처 데이터셋
- uspto-grants-1998_07
- 특허 번호
- US05786374
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