Methyl iodide → Methyl 5-fluoro-3-methyl-2-nitrobenzoate
反応式
[F:1][C:2]1[CH:3]=[C:4]([CH3:14])[C:5]([N+:11]([O-:13])=[O:12])=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].[C:15](=O)([O-])[O-].[Cs+].[Cs+].CI>CN(C=O)C.[Cl-].[Na+].O>[F:1][C:2]1[CH:3]=[C:4]([CH3:14])[C:5]([N+:11]([O-:13])=[O:12])=[C:6]([CH:10]=1)[C:7]([O:9][CH3:15])=[O:8]参加物
6
実験手順
To a solution of (E1) and cesium carbonate (1.5 eq.) in DMF (0.25 M) at RT was added methyl iodide (1.0 eq.). After the mixture was stirred for 18 h, brine was added and the mixture was extracted with EtOAc. The organic phase was dried (Na2SO4) and concentrated under reduced pressure. The yellow solid was used in the next step without purification. 1H NMR (400 MHz, DMSO, 300K) δ 7.63 (2H, m), 3.83 (3H, s), 2.29 (3H, s).
後処理
- extractionthe mixture was extracted with EtOAc
- dry with materialThe organic phase was dried (Na2SO4)
- concentrationconcentrated under reduced pressure
- customThe yellow solid was used in the next step without purification
出典と根拠
- ORDレコード
- ord-eb1d0b75953d4e298139b60ae155ebf8
- 出典データセット
- uspto-grants-2011_12
- 特許番号
- US08071623B2
反応ノート
読み込み中…