Stannous Chloride → 4-Chloro-3,5-difluorobenzene-1,2-diamine
反応式
[Cl:1][C:2]1[C:3]([F:13])=[C:4]([C:6]([N+:10]([O-])=O)=[CH:7][C:8]=1[F:9])[NH2:5].Cl[Sn]Cl>C(O)C>[Cl:1][C:2]1[C:8]([F:9])=[CH:7][C:6]([NH2:10])=[C:4]([NH2:5])[C:3]=1[F:13]参加物
4
実験手順
A solution of 348 mg (1.67 mmol) of 3-chloro-2,4-difluoro-6-nitroaniline and 1.57 g (8.28 mmol) of SnCl2 in 8 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 a red solid (285 mg, 95%), mp 77°-78° C. 1H NMR (CDCl3), 3.156 (b, 2), 3.704 (b, 2), 6.352 (dd, 1, J=1.86, 9.95).
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-d27a2da04d3042b89768c3ab9435fe12
- 出典データセット
- uspto-grants-1997_04
- 特許番号
- US05620979
反応ノート
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