Azobisisobutyronitrile → Methyl 2-(bromomethyl)-6-cyanobenzoate
반응식
[C:1]([C:3]1[CH:12]=[CH:11][CH:10]=[C:9]([CH3:13])[C:4]=1[C:5]([O:7][CH3:8])=[O:6])#[N:2].[Br:14]N1C(=O)CCC1=O.CC(N=NC(C#N)(C)C)(C#N)C>C(Cl)(Cl)Cl>[Br:14][CH2:13][C:9]1[CH:10]=[CH:11][CH:12]=[C:3]([C:1]#[N:2])[C:4]=1[C:5]([O:7][CH3:8])=[O:6]참가 물질
5
실험 절차
To a solution of EXAMPLE 6B (2.37 g) in chloroform (30 mL) was added N-bromosuccinimide (2.41 g) and AIBN (4 mg), and the mixture was heated at reflux for 18 hours. After cooling, the solvent was removed, and the concentrate was partitioned between ethyl acetate and water. The extract was washed with brine and concentrated, and the concentrate was purified by flash chromatography on silica gel with 20% ethyl acetate in hexanes.
후처리
- temperaturethe mixture was heated
- temperatureat reflux for 18 hours
- temperatureAfter cooling
- customthe solvent was removed
- customthe concentrate was partitioned between ethyl acetate and water
- washThe extract was washed with brine
- concentrationconcentrated
- customthe concentrate was purified by flash chromatography on silica gel with 20% ethyl acetate in hexanes
출처 및 근거
- ORD 기록
- ord-8fe6d4d1f682457f9724a30085ca1786
- 출처 데이터셋
- uspto-grants-2012_03
- 특허 번호
- US08143284B2
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