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Hydroquinone → Bicyclo[2.2.1]hept-2-ene-1-carbonitrile

HRID 1107996
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HRID 1107996 반응식
C1[CH:5]2[CH:6]3[CH:10]=[CH:9][CH:8]([CH:4]2C=C1)[CH2:7]3.[C:11](#[N:14])C=C.C1(C=CC(O)=CC=1)O>>[C:11]([C:6]12[CH2:7][CH:8]([CH2:4][CH2:5]1)[CH:9]=[CH:10]2)#[N:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 785HydroquinoneHCID 6492DicyclopentadieneHCID 7855Acrylonitrile

생성물 1

HCID 19737575Bicyclo[2.2.1]hept-2-ene-1-carbonitrile

실험 절차

Dicyclopentadiene of 54.2%, acrylonitrile of 45.8% and hydroquinone of 500 ppm as a polymerization inhibitor were mixed, and this mixed solution was continuously fed into a tubular reactor (inner diameter: 8 mm) at a rate of 50 ml/hr, wherein the reaction temperature was controlled to 153° C. in a residence time of the reaction solution of up to 5 hours, 170° C. in a residence time of up to 7 hours and 180° C. in a residence time of up to 9 hours. After this reaction reached a steady state, the reaction was further continued for 20 hours to obtain crude cyanonorbornene of about 1 liter having a purity of 95%. This was concentrated under reduced pressure to distill off unreacted cyclopentadiene and acrylonitrile, whereby cyanonorbornene of 950 g having a purity of 99.6% was obtained.

후처리

  1. customthis mixed solution was continuously fed into a tubular reactor
  2. customwas controlled to 153° C. in a residence time of the reaction solution
  3. customup to 5 hours
  4. wait180° C. in a residence time of up to 9 hours
  5. waitthe reaction was further continued for 20 hours

출처 및 근거

ORD 기록
ord-6f8a8bfcbcad4dd587c87618a8404805
출처 데이터셋
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06063893

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