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, 1103 mmol) in DMF (150 mL), sodium carbonate (468 g, 4415 mmol) and methyl iodide (626.63 g, 4415 mmol) were added. Resulting reaction mass was heated at 60° C. for 8 h. On completion, solid precipitated was filtered, residue washed with diethyl ether (5 times). Combined organic layers were dried, concentrated under reduced pressure giving the desired compound (302 g, 99%) which was used for further reaction.
後処理
- customResulting
- customreaction mass
- customOn completion, solid precipitated
- filtrationwas filtered
- washresidue washed with diethyl ether (5 times)
- customCombined organic layers were dried
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-878164394f97489d80a3f9fe3f7903b7
- 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…