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Dimethyl Sulfoxide → 2,5-Dichloro-3-nitrobenzoic acid

HRID 1759262
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HRID 1759262 반응식
[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9](C(O)=O)[C:8]([Cl:17])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].CS(C)=O>>[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:8]([Cl:17])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 679Dimethyl SulfoxideHCID 2809622,5-Dichloro-3-nitrobenzene-1,4-dicarboxylic acid

생성물 1

HCID 69512,5-Dichloro-3-nitrobenzoic acid

실험 절차

0.05 moles of 2,5-dichloro-3-nitro-terephthalic acid were refluxed in 2.11 moles of dimethyl sulphoxide (DMSO) at 189° C. for 70 minutes, after which the DMSO was removed by flash evaporation. The residue was dissolved in saturated sodium bicarbonate solution, which was extracted with chloroform to remove unwanted side-products. The aqueous phase was then acidified with 10% hydrochloric acid to complete precipitation and the resulting precipitate was filtered off, washed well with water and dried to give 88.5% crude yield of 2,5-dichloro-3-nitro-benzoic acid, melting at 214°-216° C.

후처리

  1. customafter which the DMSO was removed by flash evaporation
  2. dissolutionThe residue was dissolved in saturated sodium bicarbonate solution
  3. extractionwhich was extracted with chloroform
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  • customto remove unwanted side-products
  • customprecipitation
  • filtrationthe resulting precipitate was filtered off
  • washwashed well with water
  • customdried
  • 출처 및 근거

    ORD 기록
    ord-1e79ecc727d345cf963c6db09c33ab85
    출처 데이터셋
    uspto-grants-1982_07
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04339601

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