2-fluoro-3-methoxy-N-methyl-6-nitroaniline → 3-fluoro-4-methoxy-N2-methylbenzene-1,2-diamine

HRID 882204ノート

反応式

HRID 882204 の反応式
[F:1][C:2]1[C:9]([O:10][CH3:11])=[CH:8][CH:7]=[C:6]([N+:12]([O-])=O)[C:3]=1[NH:4][CH3:5]>C(O)(=O)C.[Fe]>[F:1][C:2]1[C:9]([O:10][CH3:11])=[CH:8][CH:7]=[C:6]([NH2:12])[C:3]=1[NH:4][CH3:5]

参加物

4

反応物 1

HCID 667492842-fluoro-3-methoxy-N-methyl-6-nitroaniline

生成物 1

HCID 667491243-fluoro-4-methoxy-N2-methylbenzene-1,2-diamine

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 176Acetic Acid溶媒

実験手順

A solution of 2-fluoro-3-methoxy-N-methyl-6-nitroaniline (7-2, 1.04 g, 5.20 mmol) in Acetic acid (25 ml) was charged with Iron (powder). The resulting mixture was stirred at 23 deg C. for 22 h. The reduced material concentrated in vacuo, and the residual oil was taken up in Methylene Chloride and filtered through Celite. The filtrate was again concentrated in vacuo, leaving the title compound, 3-fluoro-4-methoxy-N2-methylbenzene-1,2-diamine (7-3), as a maroon oil with >80% purity. LRMS m/z: Calc'd for C8H11FN2O (M+H) 171.2, found 170.9.

後処理

  1. concentrationThe reduced material concentrated in vacuo
  2. filtrationfiltered through Celite
  3. concentrationThe filtrate was again concentrated in vacuo

出典と根拠

ORDレコード
ord-50dac30034da4218bb8e8deced8d019b
出典データセット
uspto-grants-2015_03
特許番号
US08993779B2

反応ノート

読み込み中…