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

HRID 1414130

반응식

HRID 1414130 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 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
  4. customto remove unwanted side-products
  5. customprecipitation
  6. filtrationthe resulting precipitate was filtered off
  7. washwashed well with water
  8. customdried

출처 및 근거

ORD 기록
ord-8b7d9eb93d28423c9fd5364a70e94154
출처 데이터셋
uspto-grants-1981_02
특허 번호
US04252979

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