反応式
[CH2:1]([N:3]([CH2:19][CH3:20])[CH2:4][CH2:5][CH2:6][O:7][C:8]1[C:13]([N+:14]([O-:16])=[O:15])=[C:12](F)[CH:11]=[C:10]([F:18])[CH:9]=1)[CH3:2].C(N(CC)CC)C.[CH2:28]([NH2:32])[CH2:29][CH2:30][CH3:31]>CN(C=O)C>[CH2:28]([NH:32][C:12]1[CH:11]=[C:10]([F:18])[CH:9]=[C:8]([O:7][CH2:6][CH2:5][CH2:4][N:3]([CH2:19][CH3:20])[CH2:1][CH3:2])[C:13]=1[N+:14]([O-:16])=[O:15])[CH2:29][CH2:30][CH3:31]参加物
5
実験手順
To a stirred solution of 6-(3-diethylaminopropoxy)-2,4-difluoronitrobenzene (11 mmol) and triethylamine (22 mmol) in DMF (20 mL), a solution of n-butylamine (11 mmol) in DMF (8 mL) was added dropwise at rt, and the mixture was stirred at rt for 10 h. The reaction was quenched by cold H2O (50 mL), and the resulting mixture was extracted with EtOAc (3×100 mL). The combined EtOAc extracts were washed with brine (3×50 mL) and dried (anhydrous Na2SO4). The solvent was removed in vacuo to afford the desired 2-n-butylamino-6-(3-diethylaminopropoxy)-4-fluoronitrobenzene which was used for further transformation.
後処理
- customThe reaction was quenched by cold H2O (50 mL)
- extractionthe resulting mixture was extracted with EtOAc (3×100 mL)
- washThe combined EtOAc extracts were washed with brine (3×50 mL)
- dry with materialdried (anhydrous Na2SO4)
- customThe solvent was removed in vacuo
出典と根拠
- ORDレコード
- ord-7588175865fb4e82aef0a7b6f349f9e4
- 出典データセット
- uspto-grants-2008_04
- 特許番号
- US07361678B2
関連ノート
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