Réaction #1340568

ord-b2037b941c0f44b69c46d933a1f8181f

Équation de réaction

CC(C)(C#N)N=NC(C)(C)C#N
azobisisobutyronitrile
C=Cc1ccc(OC(C)(C)C)cc1
p-t-butoxystyrene
C=Cc1ccc(O)cc1
p-hydroxystyrene
O=S(=O)(O)O
sulfuric acid
C=Cc1ccccc1C=C
divinylbenzene
C=Cc1ccc(OC(C)(C)C)cc1
p-t-butoxystyrene
C=Cc1ccccc1
styrene
C=Cc1ccc(O)cc1.C=Cc1ccccc1.C=Cc1ccccc1C=C
divinylbenzene p-hydroxystyrene styrene

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrethe components were reacted at 90° C. for 10 hours
  2. 2
    Lavagethe mixture was washed five times with water
  3. 3
    AutreAfter isolating the ethyl acetate phase
  4. 4
    Autrethe solvent was removed

Mode opératoire

1 part by mass of divinylbenzene (manufactured by Nippon Steel Chemical Co., Ltd., purity: 57 mass %), 60 parts by mass of p-t-butoxystyrene, and 4 parts by mass of styrene were dissolved in 150 parts by mass of propylene glycol monomethyl ether. The mixture was polymerized at 70° C. for 10 hours in a nitrogen atmosphere in the presence of 4 parts by mass of azobisisobutyronitrile. After the addition of sulfuric acid to the reaction solution, the components were reacted at 90° C. for 10 hours to convert (deprotect) p-t-butoxystyrene to p-hydroxystyrene. After the addition of ethyl acetate to the resulting copolymer, the mixture was washed five times with water. After isolating the ethyl acetate phase, the solvent was removed to obtain a divinylbenzene/p-hydroxystyrene/styrene copolymer (hereinafter referred to as “resin (A-1)”). The resin (A-1) was analyzed by 13C-NMR. The resin (A-1) had a content of the structural unit (a1-1) derived from divinylbenzene of 1 mol %, a content of the structural unit (a2) derived from p-hydroxystyrene of 89 mol %, and a content of the structural unit (a3-1) derived from styrene of 10 mol %. The resin (A-1) had a polystyrene-reduced weight average molecular weight of 24,000.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08455173B2uspto-grants-2013_06