2,6-Dichloro-3-nitrotoluene → 2,4-Dichloro-m-toluidine
反応式
Cl[Sn]Cl.O.[Cl:5][C:6]1[C:11]([N+:12]([O-])=O)=[CH:10][CH:9]=[C:8]([Cl:15])[C:7]=1[CH3:16]>C(O)C>[Cl:5][C:6]1[C:11]([NH2:12])=[CH:10][CH:9]=[C:8]([Cl:15])[C:7]=1[CH3:16]参加物
4
実験手順
To a solution of SnCl2.H2O (140 g, 0.62 mol) in ethanol (350 mL) was added a solution of 2,6-dichloro-3-nitrotoluene (25 g, 0.12 mol) in ethanol (50 mL). The reaction mixture was refluxed for 1 hour. The reaction mixture was concentrated under reduced pressure. The residue was dissolved in water (100 mL), pH was adjusted to approximately pH 12 with 1N NaOH solution and extracted with ethyl acetate. The ethyl acetate layer was washed with brine, dried over sodium sulfate, and concentrated to afford 2,6-dichloro-3-aminotoluene (21 g, 98%); NMR (CDCl3) 2.42 (s, 3), 6.62 (d, 1), 7.14 (d, 1) ppm.
後処理
- temperatureThe reaction mixture was refluxed for 1 hour
- concentrationThe reaction mixture was concentrated under reduced pressure
- dissolutionThe residue was dissolved in water (100 mL)
- extractionextracted with ethyl acetate
- washThe ethyl acetate layer was washed with brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-c78937719c06435bb816f877129f639e
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07084142B2
反応ノート
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