Reaktion #1359439

Reaktionsgleichung

3-aminophthalic acid

acetic anhydride

→

3-acetamidopthalic anhydride

Ausbeute 61.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeA 1 L 3-necked round bottom flask was equipped with a mechanical stirrer
2. 2
   TemperaturThe reaction mixture was heated
3. 3
   Temperaturto reflux for 3 hours
4. 4
   FiltrationThe crystalline solid was collected by vacuum filtration
5. 5
   Waschenwashed with ether
6. 6
   SonstigeThe solid product was dried in vacua at ambient temperature to a constant weight

Vorschrift

A 1 L 3-necked round bottom flask was equipped with a mechanical stirrer, thermometer, and condenser and charged with 3-aminophthalic acid (108 g, 596 mmol) and acetic anhydride (550 mL). The reaction mixture was heated to reflux for 3 hours and cooled to ambient temperature and further to 0–5° C. for another 1 hour. The crystalline solid was collected by vacuum filtration and washed with ether. The solid product was dried in vacua at ambient temperature to a constant weight, giving 75 g (61% yield) of 3-acetamidopthalic anhydride as a white product. 1H-NMR (CDCl3) δ: 2.21 (s, 3H), 7.76 (d, 1H), 7.94 (t, 1H), 8.42 (d, 1H), 9.84 (s, 1H).

Quelle