HRID2181596

反应详情

EQUATION

反应方程式

HRID 2181596 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 added 250 g of the 2-ethyl-2-adamantyl methacrylate and p-acetoxystyrene copolymer (20:80) obtained in Synthetic Example 1, 10.3 g (0.084 mol) of 4-dimethylaminopyridine and 202 g of methanol, followed by refluxing for 20 hours. After cooling, the reaction mixture was neutralized with 7.6 g (0.126 mol) of glacial acetic acid, and the product was precipitated by pouring the reaction mixture into a large amount of water. After the precipitated polymerized product was separated by filtration and redissolved in acetone, the procedure of precipitation by pouring polymer solution into a large amount of water was repeated for a total of 3 times to purify the polymerized product. The obtained copolymer of 2-ethyl-2-adamantyl methacrylate and p-hydroxystyrene was 95.9 g. This copolymer had a weight-average molecular weight of about 8,600 with dispersion of 1.65 (GPC method; on polystyrene basis), and its copolymerization ratio was determined to be about 20:80 by a nuclear magnetic resonance (13C-NMR) analyzer. This resin was referred to as Resin A1.

WORKUP

后处理

  1. temperatureby refluxing for 20 hours
  2. temperatureAfter cooling
  3. customthe product was precipitated
  4. additionby pouring the reaction mixture into a large amount of water
  5. customAfter the precipitated polymerized product
  6. customwas separated by filtration
  7. dissolutionredissolved in acetone
  8. customthe procedure of precipitation
  9. additionby pouring polymer solution into a large amount of water
  10. customto purify the polymerized product
  11. customwith dispersion of 1.65 (GPC method; on polystyrene basis), and its copolymerization ratio