Acetic Anhydride → 4-Nitrophthalic acid anhydride

HRID 66394

反応式

HRID 66394 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([C:13]([OH:15])=[O:14])[C:7](=[CH:11][CH:12]=1)[C:8]([OH:10])=O)([O-:3])=[O:2].C(OC(=O)C)(=O)C>C(O)(=O)C>[N+:1]([C:4]1[CH:5]=[C:6]2[C:13](=[O:14])[O:15][C:8](=[O:10])[C:7]2=[CH:11][CH:12]=1)([O-:3])=[O:2]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 691211,2-Benzenedicarboxylic acid, 4-nitro-

生成物 1

HCID 2309764-Nitrophthalic acid anhydride

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 21.1 g of 4-nitrophthalic acid and 50.0 g of acetic anhydride were heated at reflux for 6 hours, following which the acetic acid was removed by distillation at atmospheric pressure. The excess acetic anhydride was removed by distillation at 15 mm Hg pressure with the flask temperature not exceeding 120° C, leaving a quantitative yield of crude 4-nitrophthalic anhydride, m.p. 114°-116° C. The product was recrystallized from chloroform to afford a 93% yield of product, m.p. 123°-124° C, identical to that of Example 1.

後処理

  1. temperaturewere heated
  2. temperatureat reflux for 6 hours
  3. customwas removed by distillation at atmospheric pressure
  4. customThe excess acetic anhydride was removed by distillation at 15 mm Hg pressure with the flask temperature not
  5. customexceeding 120° C

出典と根拠

ORDレコード
ord-acba7cf0bb274137aa2ea882011060e1
出典データセット
uspto-grants-1978_12
特許番号
US04131730

関連ノート

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