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

HRID 274514
ノート
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反応式

HRID 274514 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 144509823,4-Dihydroxy-5-nitrobenzoic acid

生成物 1

HCID 154807403,4-Diacetoxy-5-nitrobenzoic acid

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

実験手順

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°.

後処理

  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
  • 出典と根拠

    ORDレコード
    ord-f17f190c97b74fadbd38a43487a49f6c
    出典データセット
    uspto-grants-1995_02
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US05389653

    反応ノート

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