Azobisisobutyronitrile → Ethyl 2-bromo-2-(pyridin-3-yl)propanoate
反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH:7]([CH3:13])[C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:2]=1.[Br:14]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N>C(Cl)(Cl)(Cl)Cl>[Br:14][C:7]([C:3]1[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=1)([CH3:13])[C:8]([O:10][CH2:11][CH3:12])=[O:9]参加物
5
実験手順
To a stirred mixture of ethyl 2-(pyridin-3-yl)propanoate (4.2 g, 23 mmol), CCl4 (100 mL), and N-bromosuccinimide (Aldrich, 4.6 g, 26 mmol) was added 2,2′-azobisisobutyronitrile (Aldrich, 0.8 g, 5 mmol) under N2 at room temperature. The mixture was gradually heated to reflux. After 7 h, the reaction mixture was concentrated in vacuo. The crude was purified by silica gel chromatography. Mass Spec. m/z+ion 258, 260 (M+1).
後処理
- temperatureThe mixture was gradually heated to reflux
- concentrationthe reaction mixture was concentrated in vacuo
- customThe crude was purified by silica gel chromatography
出典と根拠
- ORDレコード
- ord-078b2a6d811247429c1833bc16336454
- 出典データセット
- uspto-grants-2007_08
- 特許番号
- US07253196B2
反応ノート
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