Hexane → 4-Acetoxystyrene t-butyl methacrylate benzyl methacrylate

HRID 237191

Reaction equation

HRID 237191 reaction equation
[C:1]([O:4][CH2:5][CH2:6]OCC)(=[O:3])[CH3:2].N([C:19]([CH3:25])([CH3:24])[C:20]([O:22][CH3:23])=[O:21])=N[C:12]([CH3:18])([CH3:17])[C:13]([O:15]C)=[O:14].[CH3:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31]>>[C:1]([O:4][C:5]1[CH:6]=[CH:12][C:29]([CH:28]=[CH2:27])=[CH:30][CH:31]=1)(=[O:3])[CH3:2].[C:13]([O:15][C:30]([CH3:29])([CH3:31])[CH3:1])(=[O:14])[C:12]([CH3:18])=[CH2:17].[C:20]([O:22][CH2:23][C:28]1[CH:27]=[CH:26][CH:31]=[CH:30][CH:29]=1)(=[O:21])[C:19]([CH3:24])=[CH2:25]

Participants

4

Reactant 3

HCID 8058HexaneHCID 8095Glycol monoethyl ether acetateHCID 757631,1'-Dimethyl 2,2'-(1,2-diazenediyl)bis(2-methylpropanoate)

Product 1

HCID 674157284-Acetoxystyrene t-butyl methacrylate benzyl methacrylate

Procedure

The 2-liter flask charged with 600 g of ethylene glycol monoethyl ether acetate was heated until the internal temperature of the flask became 80° C. Then, 2.30 g (0.01 mol) of polymerization initiator V-601 was added thereto and agitated for five minutes. Subsequently, the above monomer mixture solution was dropped into this solution over a period of six hours. After the completion of the dropping, the mixture was further heated and agitated for two hours. Thereafter, the reaction liquid was cooled to room temperature. After the cooling, the reaction liquid was dropped into three liters of hexane, thereby precipitating a polymer. The polymer solid was collected by filtration and dissolved in 500 g of acetone. This solution was dropped once more into three liters of hexane, and the thus obtained solid was collected by filtration and dried in vacuum. Thus, 151 g of poly(4-acetoxystyrene/t-butyl methacrylate/benzyl methacrylate) was obtained.

Workup

  1. temperaturewas heated until the internal temperature of the flask
  2. custombecame 80° C
  3. additionwas added
  4. additionSubsequently, the above monomer mixture solution was dropped into this solution over a period of six hours
  5. temperatureAfter the completion of the dropping, the mixture was further heated
  6. stirringagitated for two hours
  7. customThereafter, the reaction liquid
  8. customAfter the cooling, the reaction liquid
  9. customprecipitating a polymer
  10. filtrationThe polymer solid was collected by filtration
  11. dissolutiondissolved in 500 g of acetone
  12. additionThis solution was dropped once more into three liters of hexane
  13. filtrationthe thus obtained solid was collected by filtration
  14. customdried in vacuum

Sources & evidence

ORD record
ord-d1355ead23f14183a85e53aeb6ff943a
Source dataset
uspto-grants-2014_02
Patent number
US08642245B2

Linked notes

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