HRID1784325

反应详情

EQUATION

反应方程式

HRID 1784325 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

In a reaction vessel, 111.2 g (0.5 mol) of 3-methoxy-4-(1-ethoxyethoxy)styrene purified by distillation and 96.1 g (0.5 mol) of 4-(1-ethoxyethoxy)styrene (produced by Tosoh Corp.) were dissolved in 500 ml of dehydrated tetrahydrofuran. While stirring the resulting solution, a nitrogen gas was passed into the system and after cooling the system to −78° C., 0.02 mol of n-butyl lithium was added thereto and the polymerization was initiated. The polymerization degree was confirmed by sampling a part of the reaction solution every 30 minutes. When a desired polymerization degree was achieved, the polymerization was stopped by adding methanol to the reaction solution. After waiting until the reaction solution was cooled to room temperature, the reaction solution was added dropwise in 5 L of methanol to precipitate a polymer. The solid obtained by filtration was dissolved in 300 ml of acetone and again added dropwise in 5 L of methanol and after filtration, the solid obtained was dried under reduced pressure to obtain 153.4 g of a [3-methoxy-4-(1-ethoxyethoxy)styrene]-[4-(1-ethoxyethoxy)styrene] copolymer.

WORKUP

后处理

  1. aliquotby sampling a part of the reaction solution every 30 minutes
  2. customWhen a desired polymerization degree
  3. waitAfter waiting until the reaction solution
  4. temperaturewas cooled to room temperature
  5. customto precipitate a polymer
  6. customThe solid obtained by filtration
  7. filtrationafter filtration
  8. customthe solid obtained
  9. customwas dried under reduced pressure