Butyl Methacrylate → HCID 23469697, compound

HRID 1489301Notes

Reaction equation

HRID 1489301 reaction equation
[C:1]([O:6][CH2:7][CH:8]1[O:10][CH2:9]1)(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:11]([O:16][CH2:17][CH2:18][CH2:19][CH3:20])(=[O:15])[C:12]([CH3:14])=[CH2:13].N(C(C)(CC(OC)(C)C)C#N)=NC(C)(CC(C)(OC)C)C#N.C(S)CCCCCCCCCCC>CO.O1CCOCC1>[C:1]([O:6][CH2:7][CH:8]1[O:10][CH2:9]1)(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:11]([O:16][CH2:17][CH2:18][CH2:19][CH3:20])(=[O:15])[C:12]([CH3:14])=[CH2:13]

Participants

7

Reactant 4

HCID 7354Butyl MethacrylateHCID 7837Glycidyl methacrylateHCID 81951-DodecanethiolHCID 858672,2'-Azobis(2,4-dimethyl-4-methoxyvaleronitrile)

Product 1

HCID 23469697HCID 23469697, compoundYield 50%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 312751,4-DioxaneSolvent

Procedure

Into a 1 l four-necked flask, 25.0 g of glycidyl methacrylate, 25.0 g of n-butyl methacrylate, 10.0 g of 2,2'-azobis(4-methoxy-2,4-dimethylvaleronitrile), 5.0 g of n-dodecylmercaptan and 500 ml of dioxane were charged, dissolved and stirred. Then, stirring was continued under a nitrogen stream at 70° C. for 4 hours. The reaction solution was put into methanol to precipitate the resin. Purification was repeated with tetrahydrofuran/methanol, and then vacuum drying was conducted at 40° C. to obtain a resin powder. The obtained amount was 38.0 g. The weight average molecular weight as measured by GPC was 14,000 as calculated as polystyrene; the glass transition temperature (Tg) was 33° C.; and the epoxy equivalent was 205. 25 g of a glycidyl methacrylate/n-butyl methacrylate copolymer thus obtained, 6.5 g of an epoxy-type heat-curing agent (EX-611, manufactured by Nagase Chemicals Ltd.), 1.6 g of a curing catalyst (SI-190, manufactured by Shanshin Chemical Industry Co., Ltd.) and 77 g of diethylene glycol dimethyl ether were mixed and dissolved, followed by filtration with a 0.2 μm filter to obtain a planarizing material solution.

Workup

  1. dissolutiondissolved
  2. stirringThen, stirring
  3. customat 70° C.
  4. customfor 4 hours
  5. customto precipitate the resin
  6. customPurification
  7. customvacuum drying
  8. customwas conducted at 40° C.
  9. customto obtain a resin powder
  10. customwas 33° C.

Sources & evidence

ORD record
ord-b79e7e8e8b814e27ab0d119efc10119f
Source dataset
uspto-grants-1997_10
Patent number
US05677380

Reaction notes

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