N-(4-Bromophenyl)-2-methoxy-5-nitro-benzoic acid amide → N-(4-Bromophenyl)-2-methoxy-5-amino-benzoic acid amide
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:21])[C:10]2[CH:15]=[C:14]([N+:16]([O-])=O)[CH:13]=[CH:12][C:11]=2[O:19][CH3:20])=[CH:4][CH:3]=1>C1COCC1.[Ni]>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9](=[O:21])[C:10]2[CH:15]=[C:14]([NH2:16])[CH:13]=[CH:12][C:11]=2[O:19][CH3:20])=[CH:6][CH:7]=1参加物
4
実験手順
A mixture of N-(4-bromophenyl)-2-methoxy-5-nitro-benzoic acid amide (930 mg, 2.6 mmol) and 140 mg Ra-Ni in 40 mL THF was stirred for 20 h under an atmosphere of hydrogen (3 bar). After filtration and concentration i. vac. the subtitle compound was obtained. Yield: 890 mg (quantitative). MS [M+H]+=321 (Br-isotope pattern); TLC: Rf=0.60 (silica gel, DCM:EtOH 9:1).
後処理
- filtrationAfter filtration and concentration i
出典と根拠
- ORDレコード
- ord-6577e1dc29e54781a7bbfac0bf3aeeae
- 出典データセット
- uspto-grants-2015_02
- 特許番号
- US08951999B2
反応ノート
読み込み中…