Sulfuric Acid → 2-(2-Nitro-4-trifluoromethylphenoxy)-4,5-dichlorobenzenesulfonic acid, ammonium salt

HRID 129873

反応式

HRID 129873 の反応式
[S:1](=[O:5])(=O)([OH:3])[OH:2].[N+:6]([C:9]1[CH:23]=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:21]=[CH:20][C:10]=1[O:11][C:12]1[CH:17]=[C:16]([Cl:18])[C:15]([Cl:19])=[CH:14][CH:13]=1)([O-:8])=[O:7]>C(Cl)Cl>[NH4+:6].[N+:6]([C:9]1[CH:23]=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:21]=[CH:20][C:10]=1[O:11][C:12]1[CH:17]=[C:16]([Cl:18])[C:15]([Cl:19])=[CH:14][C:13]=1[S:1]([O-:3])(=[O:5])=[O:2])([O-:8])=[O:7]

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 13430092-(2-Nitro-4-trifluoromethylphenoxy)-4,5-dichlorobenzene

生成物 1

HCID 154073272-(2-Nitro-4-trifluoromethylphenoxy)-4,5-dichlorobenzenesulfonic acid, ammonium salt

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Fuming sulfuric acid (8 mililiter (hereinafter mL) was cooled to -20° C. and 2-(2-nitro-4-trifluoromethyl-phenoxy)-4,5-dichlorobenzene (8 g, 22.8 mmol) in methylene chloride (8 mL) was added to the solution. The mixture was stirred for 15 min and then quenched in ice. Extraction with ethyl acetate followed by flash chromatography (silica gel, methylene chloride/isopropanol/ammonium hydroxide) gave the title compound. 1H NMR (400 MHz, CD3OD) δ8.31 (d, 1H), 8.11 (s, 1H), 7.87 (dd, 1H), 7.4 (s, 1H), 7.16 (d, 1H).

後処理

  1. customquenched in ice
  2. extractionExtraction with ethyl acetate

出典と根拠

ORDレコード
ord-6859ae352e57456b9de7da9afed7fde4
出典データセット
uspto-grants-1995_11
特許番号
US05470882

関連ノート

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