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1,3-Butadiene → 1,3-Butadiene

HRID 2418781
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인쇄 미리보기

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HRID 2418781 반응식
[CH2:1]=[CH:2][CH:3]=[CH2:4].[CH3:5][O:6][C:7](=[O:19])[C:8](N=NC(C)(C)C(O)=O)([CH3:10])[CH3:9]>>[CH2:1]=[CH:2][CH:3]=[CH2:4].[CH3:5][O:6][C:7](=[O:19])[C:3]([CH3:2])([CH3:4])[C:8]([CH3:9])([CH3:10])[C:7]([O:6][CH3:5])=[O:19]
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참가 물질

4

반응물 2

HCID 78451,3-Butadiene2회HCID 21977672HCID 21977672, 화합물

생성물 2

HCID 78451,3-ButadieneHCID 11127329Dimethyl tetramethylsuccinate

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온도
80 °C

실험 절차

Preparation of the polybutadiene dicarboxylic acid dimethyl ester used in Examples 1 to 6 and in Comparison Examples II and III is carried out by the bulk polymerisation of butadiene, for which purpose 325 g of 1,3-butadiene are added under nitrogen to quantities of 55 g, 39 g, 21 g and 7 g of azo-bis-isobutyric acid methyl ester. The reaction mixture is stirred for 14 to 16 hours at 80° C., the polymerisation reaction taking place under the natural pressure of the system (around 12 bars). Thereafter the excess butadiene is distilled off. Residual butadiene and tetramethyl succinic acid dimethyl ester, formed as a secondary product, are removed over a period of 6 hours at 0.1 mbar in a rotary evaporator (bath temperature 90° C.), leaving 174 g, 140 g, 95 g and 40 g, respectively, of a crystal-clear liquid having an Mn of 800 (as determined by vapour pressure osmosis) and containing 78 mole percent of 1,4-bonds; Mn 1000 and containing 79 mole percent of 1,4-bonds; Mn 1300 and containing 80 mole percent of 1,4-bonds; Mn 6000 and containing 82 mole percent of 1,4-bonds.

후처리

  1. customthe polymerisation reaction
  2. distillationThereafter the excess butadiene is distilled off

출처 및 근거

ORD 기록
ord-1e9b6f5c5a9d4d42905b878badd80b01
출처 데이터셋
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04473686

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