Methyl iodide → 5-Bromo-1,2-dimethyl-3-nitrobenzene
反応式
[Br:1][C:2]1[CH:3]=[C:4]([N+:12]([O-:14])=[O:13])[C:5]([CH3:11])=[C:6]([CH:10]=1)[C:7](O)=O.C(=O)([O-])[O-].[Na+].[Na+].CI>CN(C=O)C>[CH3:7][C:6]1[CH:10]=[C:2]([Br:1])[CH:3]=[C:4]([N+:12]([O-:14])=[O:13])[C:5]=1[CH3:11]参加物
5
反応条件
- 温度
- 60 °C
実験手順
To a stirred solution of 5-bromo-2-methyl-3-nitrobenzoic acid (287 g, 1100 mmol) in DMF (150 mL), were added sodium carbonate (468 g, 4415 mmol) and methyl iodide (627 g, 4415 mmol). The mixture was heated at 60° C. for 8 h. The precipitate was filtered and washed with diethyl ether (5 times). The combined organic layers were dried, concentrated under reduced pressure giving the title compound (302 g, 99%) which was used directly without further purification.
後処理
- filtrationThe precipitate was filtered
- washwashed with diethyl ether (5 times)
- customThe combined organic layers were dried
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-1b8b8c030ea543b8b0eb36058fca9760
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09376422B2
反応ノート
読み込み中…