HRID262417

反应详情

EQUATION

反应方程式

HRID 262417 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A flask was equipped as in Example 1. To a solution of maleic anhydride (1.92 parts) in 4.8 parts acetone was added a solution of 1 part m-phenylenediamine, 0.32 part triethylamine and 1.6 parts acetone over a 15-minute period. A precipitate formed during that time. The heterogeneous reaction mixture was maintained at 40° C. for 30 minutes. Magnesium chloride hexahydrate (0.08 part) and 2.44 parts acetic anhydride were added all at once. The temperature was raised to 50° C. and maintained for 3 hours. After 30 minutes, the reaction mixture became homogeneous and amber in color. Five minutes later, the product began to precipitate. At the end of the reaction time, the mixture was cooled and 12 parts water added. The precipitated product was collected by vacuum filtration, washed with water, and dried for 24 hours at 60° C. in a vacuum oven. A 92% yield of N,N'-m-phenylenedimaleimide, m.p. 204°-205° C., was obtained.

WORKUP

后处理

  1. customA flask was equipped as in Example 1
  2. customA precipitate formed during that time
  3. temperatureThe temperature was raised to 50° C.
  4. temperaturemaintained for 3 hours
  5. customFive minutes
  6. customto precipitate
  7. temperatureAt the end of the reaction time, the mixture was cooled
  8. addition12 parts water added
  9. filtrationThe precipitated product was collected by vacuum filtration
  10. washwashed with water
  11. customdried for 24 hours at 60° C. in a vacuum oven