Water → 4-Trifluoromethyl-1,2-phenylenediamine
反応式
[N+:1]([C:4]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:5]=1[NH2:6])([O-])=O.Cl[Sn]Cl.O.C([O-])(O)=O.[Na+]>C(O)C>[F:12][C:11]([F:13])([F:14])[C:9]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([NH2:1])[CH:10]=1参加物
6
実験手順
A solution of 2-nitro-4-trifluoromethylaniline (5.000 g, 24.26 mmol, Aldrich, used as received) and SnCl2.2 H2O (20.00 g, 88.64 mmol, Aldrich, used as received) in absolute ethanol (50 mL) was refluxed for 45 min. It was then poured into ice (85 g) and basified with 10% aq. NaHCO3 (250 mL). The resulting suspension was extracted with ethyl acetate (400 mL). The ethyl acetate extract was dried over Na2SO4 and evaporated to give 4.14 g (87%) of pure 4-trifluoromethyl-1,2-phenylenediamine as a red powder.
後処理
- extractionThe resulting suspension was extracted with ethyl acetate (400 mL)
- extractionThe ethyl acetate extract
- dry with materialwas dried over Na2SO4
- customevaporated
出典と根拠
- ORDレコード
- ord-62109381f5f14189913bf106ba37e015
- 出典データセット
- uspto-grants-1997_04
- 特許番号
- US05622952
反応ノート
読み込み中…