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Isoprene → Styrene-isoprene-styrene

HRID 258219
ノート
印刷プレビュー

反応式

HRID 258219 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6557Isoprene2 回HCID 7501Styrene2 回HCID 1599892-Methylbuta-1,3-diene;styreneHCID 178418400CID 53628100

生成物 1

HCID 19842620Styrene-isoprene-styrene

試薬・触媒・溶媒 1

HCID 8078Cyclohexane溶媒2 回

反応条件

温度
60 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-021125ec015a4eba933b5cf5f3a0bc85
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05266394

反応ノート

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