Acetic Anhydride → 4-Nitrophthalic acid anhydride
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
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
- temperaturewere heated
- temperatureat reflux for 6 hours
- customwas removed by distillation at atmospheric pressure
- customThe excess acetic anhydride was removed by distillation at 15 mm Hg pressure with the flask temperature not
- 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
反応ノート
読み込み中…