反应 #1687675

ord-bf44012fb98d40d38f3334174e1d2dba

反应方程式

CO
methanol
C=Cc1ccc(OC(C)(C)C)cc1
p-tert-butoxystyrene
C=Cc1ccc(C)cc1
p-methylstyrene
CCC(C)(N=NC(C)(CC)C(=O)[O-])C(=O)[O-]
2,2'-azobis(methyl 2-methylpropionate)
C=Cc1ccc(C)cc1.C=Cc1ccc(OC(C)(C)C)cc1
p-tert-butoxystyrene p-methylstyrene

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他reaction in a nitrogen stream at 80° for 6 hours
  2. 2
    温度The reaction solution was cooled
  3. 3
    其他crystallization
  4. 4
    其他Precipitated crystals
  5. 5
    过滤were filtered out
  6. 6
    洗涤washed with methanol
  7. 7
    其他dried in vacuo

实验过程

To a solution of 100 g (0.567 mol) of p-tert-butoxystyrene and 3.54 g (0.03 mol) of p-methylstyrene in 300 ml of 1,4-dioxane was added a catalytic amount of 2,2'-azobis(methyl 2-methylpropionate) to carry out reaction in a nitrogen stream at 80° for 6 hours. The reaction solution was cooled and poured into 5,000 ml of a methanol solution to cause crystallization. Precipitated crystals were filtered out, washed with methanol and dried in vacuo to give 92.3 g of poly-(p-tert-butoxystyrene/p-methylstyrene)as white powder. The polymer was found to have p-tert-butoxystyrene unit and p-methylstyrene unit in a molar ratio of ca. 95:5 based on 1H NMR. The weight-average molecular weight (Mw) was determined to be about 20,000 by GPC with polystyrene calibration.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05976759uspto-grants-1999_11