2-[(2,3-Difluoro-6-nitrophenyl)amino]ethanol → 2-[(6-Amino-2,3-difluorophenyl)amino]ethanol

HRID 419931ノート

反応式

HRID 419931 の反応式
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[C:4]([N+:9]([O-])=O)[C:3]=1[NH:12][CH2:13][CH2:14][OH:15].[H][H]>C(OCC)(=O)C.C(O)C.[Pd]>[NH2:9][C:4]1[C:3]([NH:12][CH2:13][CH2:14][OH:15])=[C:2]([F:1])[C:7]([F:8])=[CH:6][CH:5]=1

参加物

6

反応物 2

HCID 579390192-[(2,3-Difluoro-6-nitrophenyl)amino]ethanolHCID 178418361HCID 178418361、化合物

生成物 1

HCID 579390152-[(6-Amino-2,3-difluorophenyl)amino]ethanol

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 2-[(2,3-difluoro-6-nitrophenyl)amino]ethanol (3.8 g, 17.4 mmol) in 70 ml of ethyl acetate and 30 ml of ethanol is added 10% Pd/C (380 mg). The reaction is shaken under 50 PSI of hydrogen for 3 hours. The pressure is periodically adjusted to 50 PSI. The reaction is filtered through celite, rinsed with ethanol and concentrated. The resulting material is used without further purification in the next step. 1H NMR (400 MHz, CDCl3) δ ppm 3.17-3.27 (m, 2H) 3.68-3.78 (m, 2H) 6.38 (ddd, J=8.89, 4.69, 2.05 Hz, 1H) 6.61-6.70 (m, 1H)

後処理

  1. filtrationThe reaction is filtered through celite
  2. washrinsed with ethanol
  3. concentrationconcentrated
  4. customThe resulting material is used without further purification in the next step

出典と根拠

ORDレコード
ord-938fcdea6a1243cd8b091fa94e5acc92
出典データセット
uspto-grants-2012_01
特許番号
US08093402B2

反応ノート

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