反応 #84028

反応方程式

3-aminophthalic acid

acetic anhydride

→

3-acetamidophthalic anhydride

収率 61.0%

反応条件

後処理

1. 1
   その他A 1 L 3-necked round bottom flask was equipped with a mechanical stirrer
2. 2
   温度The reaction mixture was heated
3. 3
   温度to reflux for 3 hours
4. 4
   ろ過The crystalline solid was collected by vacuum filtration
5. 5
   洗浄washed with ether
6. 6
   その他The solid product was dried in vacuo at ambient temperature to a constant weight

実験手順

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 about 25° C. 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 vacuo at ambient temperature to a constant weight, giving 75 g (61% yield) of 3-acetamidophthalic 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).

出典