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

HRID 1414130

反応式

HRID 1414130 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

HCID 69512,5-Dichloro-3-nitrobenzoic acid

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8b7d9eb93d28423c9fd5364a70e94154
出典データセット
uspto-grants-1981_02
特許番号
US04252979

関連ノート

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