Iodine chloride → 2-Fluoro-6-iodo-4-methylaniline
反応式
[F:1][C:2]1[CH:8]=[C:7]([CH3:9])[CH:6]=[CH:5][C:3]=1[NH2:4].O.O.O.C([O-])(=O)C.[Na+].[I:18]Cl.C(=O)(O)[O-].[Na+].S([O-])([O-])=O.[Na+].[Na+]>C(O)(=O)C.C(OCC)C>[F:1][C:2]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([I:18])[C:3]=1[NH2:4]参加物
7
実験手順
A solution of 2-fluoro-4-methylaniline (1.0 g, 8 mmol) (bought from Avocado, Lancaster or Aldrich) in glacial acetic acid (10 ml) was treated with sodium acetate trihydrate (2.2 g, 16 mmol) then iodine monochloride (1.3 g). After 30 min at room temperature aqueous sodium bicarbonate/sodium sulfite and diethyl ether were added, and the organic phase was dried (MgSO4), evaporated and chromatographed on silica eluting with 0 to 30% ethyl acetate in hexane to give the title compound, 370 mg.
後処理
- dry with materialthe organic phase was dried (MgSO4)
- customevaporated
- customchromatographed on silica eluting with 0 to 30% ethyl acetate in hexane
出典と根拠
- ORDレコード
- ord-3ba6b2ce80344eb0b87758dc93775c8e
- 出典データセット
- uspto-grants-2012_10
- 特許番号
- US08283364B2
反応ノート
読み込み中…