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 129877ノート

反応式

HRID 129877 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

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-e9744e99457643deb5db694a061563b0
出典データセット
uspto-grants-1995_11
特許番号
US05470882

反応ノート

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