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 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. The resulting reaction mixture was heated at 60° C. for 8 h. On completion, a solid precipitated was filtered, residue washed with diethyl ether (5 times). The combined organic layers were dried, concentrated under reduced pressure giving desired compound (302 g, 99%) which was used as is in subsequent steps.
後処理
- additionwere added
- customThe resulting reaction mixture
- customOn completion, a solid precipitated
- filtrationwas filtered
- washresidue washed 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-bb7a596c76d44d59a9b6360212bb2e18
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09376422B2
反応ノート
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