N-bromobutanimide → 5-Fluoro-2-iodo-4-trifluoromethyl-phenylamine
反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[C:9]([F:12])([F:11])[F:10])[NH2:5].C1C(=O)N([Br:20])C(=O)C1>C(Cl)Cl>[Br:20][C:6]1[CH:7]=[C:8]([C:9]([F:10])([F:11])[F:12])[C:2]([F:1])=[CH:3][C:4]=1[NH2:5]参加物
4
実験手順
To a stirring mixture of 3-fluoro-4-(trifluoromethyl)aniline (1.5 g) in DCM (12 mL) at room temperature was added dropwise a solution of NBS (1.5 g) in DCM (24 mL) over 15 min. The reaction mixture was stirred at rt for 1.5 h. The product mixture was concentrated under reduced pressure to one half of its original volumn. The white solid was filtered off and the crude product mixture was further purified via column chromatography. Retention time (min)=2.490, method [1], MS(ESI) 257.9 (M+H).
後処理
- concentrationThe product mixture was concentrated under reduced pressure to one half of its original volumn
- filtrationThe white solid was filtered off
- customthe crude product mixture was further purified via column chromatography
出典と根拠
- ORDレコード
- ord-e7d8c773b0a4443084e5a46a84e9f879
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09073891B2
反応ノート
読み込み中…