HRID432670

反应详情

EQUATION

反应方程式

HRID 432670 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

A mixture of homophthalic acid (200 g, 1.09 mol) and urea (80 g, 1.31 mol) was ground to a fine powder then heated at 175-185° C. until it had melted then resolidified. The mixture was cooled to ambient temperature, methanol (500 ml) was added, then the mixture was heated under reflux for 20 minutes, filtered, and allowed to cool to ambient temperature. The resulting solid was collected by filtration, washed with methanol and dried in vacuo to give homophthalimide (60 g, 34%) as a solid; m.pt. 235-240° C.; δH 4.0 (2H, s), 7.3-7.75 (3H, m), 8.10 (1H, d), 11.20 (1H, br s).

WORKUP

后处理

  1. temperatureThe mixture was cooled to ambient temperature
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 20 minutes
  4. filtrationfiltered
  5. temperatureto cool to ambient temperature
  6. filtrationThe resulting solid was collected by filtration
  7. washwashed with methanol
  8. customdried in vacuo