Acetic Anhydride → 4-Nitrophthalic acid anhydride

HRID 461621

반응식

HRID 461621 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 2309764-Nitrophthalic acid anhydride

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1d0a4b4cae294c89985cacd360cf72fc
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04064113

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