Toluene → Ethyl 4-chloro-3-nitrobenzoate
反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12].[C:14]1(C)C=CC=C[CH:15]=1>S(Cl)(Cl)=O>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH2:14][CH3:15])=[O:7])=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12]参加物
4
実験手順
4-chloro-3-nitrobenzoic acid (40.0 g, 0.2 mol) was refluxed in thionyl chloride (150 ml) for 6 hours. After cooling toluene (50 ml) was added and the mixture was evaporated to dryness. Abs. ethanol (500 ml) was added to the cooled residue, and the resulting mixture was refluxed overnight. The excess of ethanol was removed under reduced pressure and the product crystallized upon addition of aqueous sodium bicarbonate (1M). Yield: 42.5 g (93%).
後処理
- additionwas added
- customthe mixture was evaporated to dryness
- additionethanol (500 ml) was added to the cooled residue
- temperaturethe resulting mixture was refluxed overnight
- customThe excess of ethanol was removed under reduced pressure
- customthe product crystallized upon addition of aqueous sodium bicarbonate (1M)
出典と根拠
- ORDレコード
- ord-845d090488194370a30c5357d06afd4a
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06710044B2
反応ノート
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