Dichloromethane → 5-Bromo-2,3-dimethoxypyridine
反応式
[CH3:1][O:2][C:3]1[C:8]([O:9][CH3:10])=[CH:7][CH:6]=[CH:5][N:4]=1.C(Cl)Cl.[Br:14]Br>C([O-])(O)=O.[Na+]>[Br:14][C:6]1[CH:7]=[C:8]([O:9][CH3:10])[C:3]([O:2][CH3:1])=[N:4][CH:5]=1参加物
5
実験手順
To a 100 mL round-bottomed flask was added 2,3-dimethoxypyridine (2 mL, 15 mmol, Alfa Aesar, Ward Hill, Mass.), CH2Cl2 (30 mL), and bromine (0.7 mL, 14 mmol). The reaction mixture was stirred at rt for 16 h. The reaction mixture was then diluted with sat. NaHCO3 (30 mL) and extracted with EtOAc (2×50 mL). The combined organic extracts were washed with sat. NaCl (20 mL), dried over Na2SO4, filtered and concentrated. Purification by silica gel chromatography (50% CH2Cl2/hexanes) afforded the title compound (1.98 g, 60%). MS (ESI, positive ion) m/z: 218 (M(79Br)+1).
後処理
- extractionextracted with EtOAc (2×50 mL)
- washThe combined organic extracts were washed with sat. NaCl (20 mL)
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customPurification by silica gel chromatography (50% CH2Cl2/hexanes)
出典と根拠
- ORDレコード
- ord-08016a45d69e42e1b8eee1f95839037d
- 出典データセット
- uspto-grants-2010_10
- 特許番号
- US07820665B2
反応ノート
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