N-benzyl-2-nitroaniline → N1-Benzylbenzene-1,2-diamine
反応式
[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[N+:15]([O-])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C(O)(=O)C.[Fe]>[CH2:1]([NH:8][C:9]1[C:10]([NH2:15])=[CH:11][CH:12]=[CH:13][CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1参加物
4
反応条件
- 温度
- 40 °C
実験手順
To a solution of Benzyl-(2-nitro-phenyl)-amine (230 mg, 1 mmol) in 3 ml acetic acid, was added iron (70 mg, 1.24 mmol). The reaction mixture was heated to 40° C. under argon for 2 hours. The mixture was cooled to ambient temperature and filtered through celite and the filtrate was concentrated. The resulting solid was dissolved in ethyl acetate. The organic layer was washed with saturated NaHCO3, dried over MgSO4, filtered and the filtrate was concentrated in vacuo to yield crude product that was used in step Example 5c.
後処理
- temperatureThe mixture was cooled to ambient temperature
- filtrationfiltered through celite
- concentrationthe filtrate was concentrated
- dissolutionThe resulting solid was dissolved in ethyl acetate
- washThe organic layer was washed with saturated NaHCO3
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationthe filtrate was concentrated in vacuo
- customto yield crude product that
出典と根拠
- ORDレコード
- ord-d0ed86af5dc04a5d9adfa9cb8722f05b
- 出典データセット
- uspto-grants-2010_02
- 特許番号
- US07662581B1
反応ノート
読み込み中…