3-Fluoro-2-nitro-N-phenylaniline → HCID 44254861、化合物
反応式
[F:1][C:2]1[C:3]([N+:15]([O-])=O)=[C:4]([NH:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:5]=[CH:6][CH:7]=1>CCOC(C)=O.[Pd]>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([NH:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:3]=1[NH2:15]参加物
4
実験手順
A mixture of (3-fluoro-2-nitrophenyl)phenylamine (1.06 g, 4.56 mmol) and 10% Pd/C (100 mg) in EtOAc (20 mL) was degassed with a stream of nitrogen and stirred at RT under a hydrogen atmosphere for 7 h. The suspension was then filtered through a PTFE frit and the filtrate was concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, gradient 0-20% EtOAc in cyclohexane) affording 3-Fluoro-N1-phenylbenzene-1,2-diamine (440 mg, 48%). LCMS: RT 3.46 min [M+H]+ 203.1.
後処理
- customwas degassed with a stream of nitrogen
- filtrationThe suspension was then filtered through a PTFE frit
- concentrationthe filtrate was concentrated in vacuo
- customThe resulting residue was purified by column chromatography (Si—PCC, gradient 0-20% EtOAc in cyclohexane)
出典と根拠
- ORDレコード
- ord-7a3764df5e804b42a16b1c4e575ab2b6
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08653089B2
反応ノート
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