Sodium Chloride → N-tert-Butyl-2-nitroaniline
反応式
F[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[C:11]([NH2:15])([CH3:14])([CH3:13])[CH3:12].[Cl-].[Na+]>CN(C)C=O>[C:11]([NH:15][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9])([CH3:14])([CH3:13])[CH3:12]参加物
5
実験手順
To a solution of 1-fluoro-2-nitro-benzene (1 g, 7.1 mmol) in dimethylformamide (15 mL) was added tert-butyl amine (0.82 mL, 7.81 mmol) at room temperature, and the reaction mixture stirred for 12 hours at room temperature under nitrogen. Upon completion, the reaction mixture was poured into a saturated aqueous solution of sodium chloride (50 mL) and extracted with ethyl acetate (50 mL). The organic layer was dried over anhydrous sodium sulfate, concentrated in vacuo, and the residue was purified via flash column chromatography (silica, 1% ethyl acetate in hexane) to give tert-butyl-(2-nitrophenyl)-amine as an orange oil. MS (ES) m/z 195.2
後処理
- extractionextracted with ethyl acetate (50 mL)
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
- customthe residue was purified via flash column chromatography (silica, 1% ethyl acetate in hexane)
出典と根拠
- ORDレコード
- ord-203045e470a64bd19e18d29810cf970e
- 出典データセット
- uspto-grants-2009_04
- 特許番号
- US07517899B2
反応ノート
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