Acetic Anhydride → 4-Nitrophthalic acid anhydride

HRID 66394

Reaktionsgleichung

Reaktionsgleichung von HRID 66394
[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]

Komponenten

4

Edukt 2

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

Produkt 1

HCID 2309764-Nitrophthalic acid anhydride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-acba7cf0bb274137aa2ea882011060e1
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04131730

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