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Isoprene → Styrene-isoprene-styrene

HRID 258219
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HRID 258219 반응식
[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C([Li])(CC)C.[CH2:14]=[CH:15][C:16](=[CH2:18])[CH3:17].C=CC(=C)C.[CH2:24]=[CH:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>C1CCCCC1>[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH2:14]=[CH:15][C:16](=[CH2:17])[CH3:18].[CH2:24]=[CH:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6557Isoprene2회HCID 7501Styrene2회HCID 1599892-Methylbuta-1,3-diene;styreneHCID 178418400CID 53628100

생성물 1

HCID 19842620Styrene-isoprene-styrene

시약·촉매·용매 1

HCID 8078Cyclohexane용매2회

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온도
60 °C

실험 절차

To a 2.6 liter autoclave were charged 1900 ml of cyclohexane and 88.1 gm of styrene monomer. The mixture was heated to 60° C. and 3.7 ml of a 1.4 molar solution of sec-butyllithium initiator in cyclohexane was added. After 40 minutes, when analysis of the reaction mixture indicated that polymerization of the styrene monomer was complete, the reaction temperature was reduced to 50° C., and 116.7 gm of isoprene was added. After 45 minutes, no unreacted isoprene was detected. The living styrene-isoprene diblock polymer was then coupled to form a styrene-isoprene-styrene triblock polymer by adding 32.0 ml of 0.12M 1,2-dibromoethane in cyclohexane over a period of 11 minutes. Analysis of the product by gel-permeation chromatography (GPC) indicated that the triblock polymer had a peak molecular weight of 76,800, and contained approximately 12% residual diblock. From the proton NMR spectrum of the product, it was determined that it contained 41.7 wt. % styrene. The solvent was removed from the polymer solution under vacuum at 90° C.

후처리

  1. customwas reduced to 50° C.
  2. waitAfter 45 minutes

출처 및 근거

ORD 기록
ord-021125ec015a4eba933b5cf5f3a0bc85
출처 데이터셋
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05266394

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