Stannous Chloride → N,N-dimethyl-m-phenylenediamine
反応式
[CH3:1][N:2]([CH3:12])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([N+:9]([O-])=O)[CH:4]=1.[Sn](Cl)Cl>C(O)C>[CH3:1][N:2]([CH3:12])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([NH2:9])[CH:4]=1参加物
4
実験手順
N,N-dimethyl-3-nitroaniline (3.00 g, 18.1 mmol) was dissolved in ethanol (40 cm3). Tin dichloride (16.3 g, 72.0 mmol) was added and the reaction heated under reflux for 16 h. The reaction mixture was allowed to cool before the bulk of the solvent was removed under reduced pressure. The remaining residue was poured in to water (100 cm3), and basified with sodium hydroxide (3M). The mixture was extracted with chloroform (3×30 cm3). The combined extracts were dried over sodium sulphate, filtered and the solvent removed under reduced pressure to give the product as a brown oil (2.01 g, 82%).
後処理
- temperaturethe reaction heated
- temperatureunder reflux for 16 h
- temperatureto cool before the bulk of the solvent
- customwas removed under reduced pressure
- additionThe remaining residue was poured in to water (100 cm3)
- extractionThe mixture was extracted with chloroform (3×30 cm3)
- dry with materialThe combined extracts were dried over sodium sulphate
- filtrationfiltered
- customthe solvent removed under reduced pressure
出典と根拠
- ORDレコード
- ord-971757b34e2e402bbe2718b62e4a1ffd
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08658665B2
反応ノート
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