Sulfuric Acid → HCID 86643781, compound

HRID 1253386Notes

Reaction equation

HRID 1253386 reaction equation
[CH:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH:9]=[CH2:10])=[CH2:2].C([O:15][C:16]1[CH:23]=[CH:22][C:19]([CH:20]=[CH2:21])=[CH:18][CH:17]=1)(C)(C)C.[CH2:24]=[CH:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1.N(C(C)(C)C#N)=NC(C)(C)C#N.S(=O)(=O)(O)O.OC1C=CC(C=C)=CC=1>COCC(O)C.C(OCC)(=O)C>[CH:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH:9]=[CH2:10])=[CH2:2].[OH:15][C:16]1[CH:23]=[CH:22][C:19]([CH:20]=[CH2:21])=[CH:18][CH:17]=1.[CH2:24]=[CH:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1

Participants

9

Reactant 6

HCID 1118Sulfuric AcidHCID 6547AzobisisobutyronitrileHCID 7501StyreneHCID 624534-VinylphenolHCID 666661,2-DiethenylbenzeneHCID 5775311-(Tert-butoxy)-4-ethenylbenzene2×

Product 1

HCID 86643781HCID 86643781, compound

Reagents, catalysts & solvents 2

HCID 79001-Methoxy-2-propanolSolventHCID 8857Ethyl AcetateSolvent

Procedure

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.

Workup

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

Sources & evidence

ORD record
ord-b2037b941c0f44b69c46d933a1f8181f
Source dataset
uspto-grants-2013_06
Patent number
US08455173B2

Reaction notes

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