1-Methanesulfonyl-3-nitro-5-trifluoromethylbenzene → 3-Methanesulfonyl-5-(trifluoromethyl)aniline
反応式
[CH3:1][S:2]([C:5]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[C:7]([N+:15]([O-])=O)[CH:6]=1)(=[O:4])=[O:3]>CO.[Pd]>[CH3:1][S:2]([C:5]1[CH:6]=[C:7]([CH:8]=[C:9]([C:11]([F:12])([F:13])[F:14])[CH:10]=1)[NH2:15])(=[O:4])=[O:3]参加物
4
実験手順
Stir the mixture of 1-(methylsulfonyl)-3-nitro-5-(trifluoromethyl)benzene (2 g, 7.43 mmol), Pd/C (10%, 500 mg) in methanol (100 mL) under hydrogen atmosphere at room temperature for 15 hrs. Filter off the solid and concentrate the filtrate under reduced pressure. Purify the residue with flash chromatography (silica gel, EtOAc:PE=1:5) to afford the desired product (1.3 g, 73%). MS: (M+23): 262.0.
後処理
- filtrationFilter off the solid
- concentrationconcentrate the filtrate under reduced pressure
- customPurify the residue with flash chromatography (silica gel, EtOAc:PE=1:5)
出典と根拠
- ORDレコード
- ord-ef311f5d17df41ff838e414a251bdca7
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09359338B2
反応ノート
読み込み中…