3,5-Bis(trifluoromethyl)phenyl isocyanate → 2-[2-[3-[3,5-Bis(trifluoromethyl)phenyl]ureido]-4-trifluoromethylphenoxy]-5-(1,1-dimethylpropyl)benzenesulfonic acid, ammonium salt

HRID 129878ノート

反応式

HRID 129878 の反応式
[NH2:1][C:2]1[CH:23]=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:21]=[CH:20][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]([CH3:15])([CH3:14])[CH2:12][CH3:13])=[CH:7][C:6]=1[S:16]([OH:19])(=[O:18])=[O:17].[F:28][C:29]([F:44])([F:43])[C:30]1[CH:31]=[C:32]([N:40]=[C:41]=[O:42])[CH:33]=[C:34]([C:36]([F:39])([F:38])[F:37])[CH:35]=1>N1C=CC=CC=1>[NH4+:1].[F:28][C:29]([F:43])([F:44])[C:30]1[CH:31]=[C:32]([NH:40][C:41](=[O:42])[NH:1][C:2]2[CH:23]=[C:22]([C:24]([F:27])([F:25])[F:26])[CH:21]=[CH:20][C:3]=2[O:4][C:5]2[CH:10]=[CH:9][C:8]([C:11]([CH3:14])([CH3:15])[CH2:12][CH3:13])=[CH:7][C:6]=2[S:16]([O-:19])(=[O:18])=[O:17])[CH:33]=[C:34]([C:36]([F:39])([F:37])[F:38])[CH:35]=1

参加物

4

反応物 2

HCID 27333143,5-Bis(trifluoromethyl)phenyl isocyanateHCID 99091322-(2-Amino-4-trifluoromethylphenoxy)-5-(1,1-dimethylpropyl)benzenesulfonic acid

生成物 1

HCID 1317192132-[2-[3-[3,5-Bis(trifluoromethyl)phenyl]ureido]-4-trifluoromethylphenoxy]-5-(1,1-dimethylpropyl)benzenesulfonic acid, ammonium salt

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

2-(2-Amino-4-trifluoromethylphenoxy)-5-(1,1-dimethylpropyl)benzenesulfonic acid (260 mg, 0.0006 mol) and 3,5-bis(trifluoromethyl)phenyl isocyanate (130.9 ml, 0.0005 mol) were mixed in pyridine (5 ml), under argon, for sixteen hours at room temperature. The solvent was evaporated and the residue flash chromatographed (silica gel, methylene chloride/isopropanol/ammonium hydroxide), dried and evaporated to give the title compound. 1H NMR (250 MHz, DMSO) ∂9.20 (s, 1H), 8.90 (s, 1H), 7.90 (s, 1H), 7.50 (s, 2H), 7.25 (d, 1H), 7.05 (s, 1H), 6.80-6.30 (m, 4H), 1.0 (q, 3H), 0.065 (s, 6H), 0.045 (d, 2H).

後処理

  1. customThe solvent was evaporated
  2. customthe residue flash chromatographed (silica gel, methylene chloride/isopropanol/ammonium hydroxide)
  3. customdried
  4. customevaporated

出典と根拠

ORDレコード
ord-d9f93a8a22684b8caca1c3ff7498a6a4
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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