HRID1160024

反应详情

EQUATION

反应方程式

HRID 1160024 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

5-norbornene-2-allylacetate (5 mL, 30.9 mmol), 5-butylnorbornene (1.2 mL, 6.6 mmol), 5-norbornene-2-carboxylic methylester (1 mL, 6.6 mmol) and toluene (12.4 mL) were charged into a 250 mL Schlenk flask. Pd(OAc)2 (0.66 mg, 2.94 μmol) and [(Cy)3PH][(B(C6F5)4) (5.65 mg, 5.88 μmol) were dissolved in CH2Cl2 (1 mL) and added to the monomer solution. While the reaction mixture was stirred for 18 hours at 90° C., the reaction mixture became viscous. After the reaction was completed, 120 ml of toluene was added to the viscous solution to dilute it. The solution was poured into an excess of ethanol to precipitate a white polymer, which was filtered through a glass funnel, washed with ethanol, and dried in vacuo at 80° C. for 24 hours to yield 5-norbornene-2-allylacetate/5-butylnorbornene/5-norbornene-2-carboxylic methylester polymer (6.45 g: 90.5% by weight based on the total weight of used monomers). The weight average molecular weight (Mw) of the polymer was 211,891 and Mw/Mn was 2.67.

WORKUP

后处理

  1. additionadded to the monomer solution
  2. additionto dilute it
  3. customto precipitate a white polymer, which
  4. filtrationwas filtered through a glass funnel
  5. washwashed with ethanol
  6. customdried in vacuo at 80° C. for 24 hours