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3,4-Dihydroxy-5-nitrobenzoic acid → 3,4-Diacetoxy-5-nitrobenzoic acid

HRID 725382
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HRID 725382 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[C:10]=1[OH:11])[C:5]([OH:7])=[O:6]>C(OC(=O)C)(=O)C>[C:2]([O:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[C:10]=1[O:11][C:5](=[O:6])[CH3:4])[C:5]([OH:7])=[O:6])(=[O:1])[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 144509823,4-Dihydroxy-5-nitrobenzoic acid

생성물 1

HCID 154807403,4-Diacetoxy-5-nitrobenzoic acid

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

7.3 g of 3,4-dihydroxy-5-nitrobenzoic acid are treated with 30 ml of acetic anhydride, whereupon the mixture is held at the reflux temperature for 8 hours. The reaction mixture is poured on to ice. The separated precipitate is filtered under suction, washed with water and taken up in methylene chloride. The organic phase is dried over sodium sulfate and evaporated. The residue obtained is recrystallized from methylene chloride/n-hexane in the cold. There is obtained 3,4-diacetoxy-5-nitrobenzoic acid in the form of colorless crystals of m.p. 126°-127°.

후처리

  1. additionThe reaction mixture is poured on to ice
  2. filtration
The separated precipitate is filtered under suction
  • washwashed with water
  • dry with materialThe organic phase is dried over sodium sulfate
  • customevaporated
  • customThe residue obtained
  • customis recrystallized from methylene chloride/n-hexane in the cold
  • 출처 및 근거

    ORD 기록
    ord-9e863ff076164799b968fd3bb4f3a7e9
    출처 데이터셋
    uspto-grants-1998_01
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05705703

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