HRID2120032

反应详情

EQUATION

反应方程式

HRID 2120032 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into a flask were charged 250 g of the copolymer of 2-ethyl-2-adamantyl methacrylate and p-acetoxystyrene (20:80) obtained in Reference Example 5, 10.3 g (0.084 mol) of 4-dimethylaminopyridine and 202 g of methanol and the mixture was aged for 20 hours under reflux. After cooling, the reaction solution was neutralized with 7.6 g (0.126 mol) of glacial acetic acid, and precipitated by pouring into a large amount of water. The precipitated polymer was filtrated, and dissolved in acetone. The resulted solution was poured into a large amount of water to cause precipitation. This operation was repeated three times in total, to effect purification. The amount of the resulted copolymer of 2-ethyl-2-adamentyl methacrylate and p-hydroxystyrene was 95.9 g. The weight-average molecular weight was about 8600, the degree of dispersion was 1.65 (GPC method: reduced by polystyrene), and the copolymerization ratio was determined to be about 20:80 by a nuclear magnetic resonance (13C-NMR) spectrometer. This resin is called resin A5.

WORKUP

后处理

  1. temperatureunder reflux
  2. temperatureAfter cooling
  3. customprecipitated
  4. additionby pouring into a large amount of water
  5. filtrationThe precipitated polymer was filtrated
  6. dissolutiondissolved in acetone
  7. additionThe resulted solution was poured into a large amount of water
  8. customprecipitation
  9. custompurification