Stannous Chloride → 4,5-Bis(trifluoromethyl)benzene-1,2-diamine
反応式
[F:1][C:2]([F:18])([F:17])[C:3]1[C:9]([C:10]([F:13])([F:12])[F:11])=[CH:8][C:6]([NH2:7])=[C:5]([N+:14]([O-])=O)[CH:4]=1.Cl[Sn]Cl>C(O)C>[F:1][C:2]([F:17])([F:18])[C:3]1[C:9]([C:10]([F:13])([F:12])[F:11])=[CH:8][C:6]([NH2:7])=[C:5]([NH2:14])[CH:4]=1参加物
4
実験手順
A solution of 122 mg (0.445 mmol) of 4,5-bis(trifluoromethyl)-2-nitroaniline and 498 mg (2.62 mmol) of SnCl2 in 6 mL of ethanol was heated at 70° C. for 2 h. The solution was evaporated to remove the ethanol. The residue was treated with 2N NaOH to pH=13. White precipitate was observed. The mixture was extracted by CHCl3 (3×10 mL). The extract was dried (MgSO4) and evaporated to leave 102 mg (94%) of oil. 1H NMR (CDCl3), 3.70 (mb, 4), 7.069 (s, 2) and some impurity. 19F NMR (CDCl3), 56.659 (s).
後処理
- customThe solution was evaporated
- customto remove the ethanol
- additionThe residue was treated with 2N NaOH to pH=13
- extractionThe mixture was extracted by CHCl3 (3×10 mL)
- dry with materialThe extract was dried (MgSO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-3f6d420159344002bd7d371c98f04cc7
- 出典データセット
- uspto-grants-1996_05
- 特許番号
- US05514680
反応ノート
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