HRID868689

反应详情

EQUATION

反应方程式

HRID 868689 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A glass flask having an inner volume of 3 liters was fitted with a theremometer, a stirrer and a water separater. This reactor was charged with 240 g of a xylene solution containing 120 g of maleic anhydride. Then, a solution of 220 g of dodecylamine in 1880 g of xylene was added thereto gradually and piecemeal at 40° C. over a period of 120 minutes. After the addition was completed, the resultant mixture and 65.4 g of ortho-phosphoric acid (purity 89% by weight), 0.672 g of p-methoxyphenol, and 0.05 g of zinc acetate added thereto were heated at 150° C. for four hours to effect reaction. Thereafter, the resultant reaction mixture was cooled to 30° C., washed with 400 ml of water, and separated into a water layer and a xylene layer. The xylene layer was filtered to effect removal of insolubles. The xylene layer now free from insolubles was distilled to expel xylene. Consequently there was obtained 260 g of slightly impure N-dodecyl maleimide. It was found to have purity of 91.2% by weight, indicating the yield thereof to be 75.3 mol % based on dodecylamine.

WORKUP

后处理

  1. customA glass flask having
  2. customan inner volume of 3 liters was fitted with a theremometer, a stirrer
  3. additionAfter the addition
  4. customreaction
  5. customThereafter, the resultant reaction mixture
  6. temperaturewas cooled to 30° C.
  7. washwashed with 400 ml of water
  8. customseparated into a water layer
  9. filtrationThe xylene layer was filtered
  10. customremoval of insolubles
  11. distillationThe xylene layer now free from insolubles was distilled