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

HRID 129873

반응식

HRID 129873 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  1. customquenched in ice
  2. extractionExtraction with ethyl acetate

출처 및 근거

ORD 기록
ord-6859ae352e57456b9de7da9afed7fde4
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05470882

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