2-(2-Nitro-4-trifluoromethylphenoxy)-5-(1,1-dimethylpropyl)benzenesulfonic acid, ammonium salt → 2-(2-Amino-4-trifluoromethylphenoxy)-5-(1,1-dimethylpropyl)benzenesulfonic acid

HRID 1416352ノート

反応式

HRID 1416352 の反応式
[NH4+].[N+:2]([C:5]1[CH:26]=[C:25]([C:27]([F:30])([F:29])[F:28])[CH:24]=[CH:23][C:6]=1[O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]([CH3:18])([CH3:17])[CH2:15][CH3:16])=[CH:10][C:9]=1[S:19]([O-:22])(=[O:21])=[O:20])([O-])=O>C(OCC)(=O)C.[Pd]>[NH2:2][C:5]1[CH:26]=[C:25]([C:27]([F:30])([F:28])[F:29])[CH:24]=[CH:23][C:6]=1[O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]([CH3:17])([CH3:18])[CH2:15][CH3:16])=[CH:10][C:9]=1[S:19]([OH:22])(=[O:21])=[O:20]

参加物

4

反応物 1

HCID 1317192122-(2-Nitro-4-trifluoromethylphenoxy)-5-(1,1-dimethylpropyl)benzenesulfonic acid, ammonium salt

生成物 1

HCID 99091322-(2-Amino-4-trifluoromethylphenoxy)-5-(1,1-dimethylpropyl)benzenesulfonic acid

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

2-(2-Nitro-4-trifluoromethylphenoxy)-5-(1,1-dimethylpropyl)benzenesulfonic acid, ammonium salt (620 mg) was mixed in ethyl acetate (50 ml) and palladium on carbon (202 mg) was added under argon. The mixture was hydrogenated in a Parr bottle at 55 psi for two hours. The sample was filtered to remove the catalyst, mixed with methanol and degassed for several hours to yield the title compound. 1H NMR (250 MHz, CD3OD) ∂ 7.95 (d, 1H), 7.30 (dd, 1H), 7.05 (dd, 2H), 6.85 (dd, 1H), 6.75 (d, 1H), 1.65 (q, 3H), 1.25 (s, 6H), 0.65 (t, 2H).

後処理

  1. filtrationThe sample was filtered
  2. customto remove the catalyst
  3. additionmixed with methanol
  4. customdegassed for several hours

出典と根拠

ORDレコード
ord-9c17cef3614b437999b62fbc8ac438f2
出典データセット
uspto-grants-1999_06
特許番号
US05912270

反応ノート

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