HRID1658154

反应详情

EQUATION

反应方程式

HRID 1658154 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A solution of 250 g of copoly(styrene-maleic anhydride (commercially available from the Monsanto Chemical Company under the tradename of Lytron 810) in 2500 ml of dry dimethylformamide is made by stirring in a 5-liter flask, containing a reflux condenser, thermometer, stirrer, and dropping funnel. The mixture is heated to 110°C and 230 g of N,N-dimethyl-1,3-propanediamine is added slowly at a rate to keep the mixture boiling slightly. Polymer precipitates as a gummy mass at first but goes back into solution after about half of the amine is added. The condenser is replaced by a distillation column and about 500 ml of material is removed by distillation with stirring. The residue is cooled, precipitated in water, collected by filtration and air-dried at room temperature for 2 days. The solid is dissolved in acetone, and again precipitated in water and air-dried. Yield = 260 g of off-white, friable solid.

WORKUP

后处理

  1. additioncontaining a reflux condenser
  2. customthermometer, stirrer, and dropping
  3. customPolymer precipitates as a gummy mass at first but
  4. additionis added
  5. distillationThe condenser is replaced by a distillation column and about 500 ml of material
  6. customis removed by distillation
  7. stirringwith stirring
  8. temperatureThe residue is cooled
  9. customprecipitated in water
  10. filtrationcollected by filtration
  11. customair-dried at room temperature for 2 days
  12. dissolutionThe solid is dissolved in acetone
  13. customagain precipitated in water
  14. customair-dried