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Acrylic Acid → 5-Phenyl-2,4-pentadienoic acid

HRID 434545
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인쇄 미리보기

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HRID 434545 반응식
[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(C1C=CC=CC=1)C.[C:17]([OH:21])(=[O:20])[CH:18]=[CH2:19].C(OOC(C)(C)C)(=O)C.C([O-])(=O)CCCCCC(C)(C)C>C(C(C)=O)C>[CH:1]([CH:19]=[CH:18][C:17]([OH:21])=[O:20])=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 6581Acrylic Acid3회HCID 7500EthylbenzeneHCID 7501StyreneHCID 61019tert-Butyl peroxyacetate2회HCID 21225528Neodecanoate

생성물 1

HCID 737775-Phenyl-2,4-pentadienoic acid수율 446.8%

시약·촉매·용매 1

HCID 6569
Methyl Ethyl Ketone
용매
2회

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온도
85 °C

실험 절차

Into a polymerization reactor equipped with an agitator and a reflux condenser were charged 580 grams of styrene, 3.0 grams of terpenolene and 200 ml of ethylbenzene. Then 80 grams of high cis-polybutadiene from Goodyear Tire & Rubber Company (Budene 1208) was dissolved in the mixture. After the rubber had dissolved, a solution of 40 grams of acrylic acid in 60 ml of methyl ethyl ketone (335 ml) was introduced into the mixture. The temperature of the reaction mixture was raised to 85° C. and maintained at this level during the ensuing polymerization. Polymerization was initiated by introducing into the system a mixture of 0.2 ml of tert-butyl peracetate and 0.2 ml of tert-butyl per-neo-decanoate. One hour later, continuous addition of a solution of 40 grams of acrylic acid and 60 ml of methyl ethyl ketone was initiated and this addition was continued over a four hour period. At one hour and again at four hours after the start of the continuous addition of the acrylic acid solution, additional 0.2 ml portions of tert-butyl peracetate were introduced into the polymerization mixture. Polymerization was terminated 5.5 hours after initiation and the resultant polymer was recovered and dried, first in air and then in a vacuum oven, to yield 432 grams of rubber-modified styrene-acrylic acid graft copolymer. In order to produce enough copolymer for the compounding and ensuing test work this polymerization procedure was repeated four more times and the products from the five runs were combined and mixed in a Waring blender. The resultant polymer contained about 84.2 weight percent styrene and about 15.8 weight percent acrylic acid. Its rubber content was approximately 18.5 percent based on the weight of the resin phase.

후처리

  1. customInto a polymerization reactor equipped with an agitator and a reflux condenser
  2. dissolutionAfter the rubber had dissolved
  3. temperaturemaintained at this level during the ensuing polymerization
  4. customPolymerization
  5. additionby introducing into the system
  6. additionthis addition
  7. waitAt one hour
  8. additionwere introduced into the polymerization mixture
  9. customPolymerization
  10. customwas terminated 5.5 hours after initiation
  11. customthe resultant polymer was recovered
  12. customdried, first in air

출처 및 근거

ORD 기록
ord-ced5ea2d098b405d8634d1214109fc2f
출처 데이터셋
uspto-grants-1983_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04397986

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