Methyl iodide → 1-Bromo-5-fluoro-4-methoxy-2-nitrobenzene
反応式
[Br:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([OH:11])=[C:4]([F:12])[CH:3]=1.[C:13](=O)([O-])[O-].[K+].[K+].CI>CN(C=O)C>[CH3:13][O:11][C:5]1[CH:6]=[C:7]([N+:8]([O-:10])=[O:9])[C:2]([Br:1])=[CH:3][C:4]=1[F:12]参加物
5
実験手順
A solution of 4-bromo-2-fluoro-5-nitrophenol (25 g, 106 mmol) in DMF (200 mL) was treated with potassium carbonate (28.9 g, 212 mmol) and methyl iodide (12.8 mL, 212 mmol). The reaction mixture was stirred at 60 C for 5 hours and evaporated in vacuo. The mixture was partitioned between water and ethyl acetate. The organic layer was dried over magnesium sulfate and evaporated under vacuum to afford the product (25.6 g, 97%) as a yellow solid. LC-MS (ES) (M+H)+ m/z=251.
後処理
- customevaporated in vacuo
- customThe mixture was partitioned between water and ethyl acetate
- dry with materialThe organic layer was dried over magnesium sulfate
- customevaporated under vacuum
出典と根拠
- ORDレコード
- ord-0a3df1d3f7944ced89caa6387a12a789
- 出典データセット
- uspto-grants-2010_04
- 特許番号
- US07691850B2
反応ノート
読み込み中…