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Carbon Tetrachloride → Ethyl 2-[4-(2,2-dichlorovinyl)phenyl]propionate

HRID 637610
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인쇄 미리보기

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HRID 637610 반응식
[CH:1]([C:3]1[CH:8]=[CH:7][C:6]([CH:9]([CH3:15])[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:5][CH:4]=1)=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CCCCCC.C(OCC)(=O)C.[C:47](Cl)(Cl)([Cl:49])[Cl:48]>>[Cl:48][C:47]([Cl:49])=[CH:1][C:3]1[CH:8]=[CH:7][C:6]([CH:9]([CH3:15])[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:5][CH:4]=1
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참가 물질

6

반응물 5

HCID 5943Carbon TetrachlorideHCID 8058Hexane2회HCID 8857Ethyl AcetateHCID 11776TriphenylphosphineHCID 13066570rac 2-(4-Formylphenyl)propionic Acid Ethyl Ester

생성물 1

HCID 13388016Ethyl 2-[4-(2,2-dichlorovinyl)phenyl]propionate

반응 조건

온도
50 °C

실험 절차

In 260 ml of carbon tetrachloride were dissolved 60 g of ethyl 2-(4-formylphenyl)propionate and 122 g of triphenylphosphine, followed by stirring in a stream of nitrogen gas at 50° C. for 4.5 hours. After cooling, the mixture was poured into 1 l of cold n-hexane and filtered. The filtrate was concentrated under reduced pressure to give an oily substance, which was subjected to silica gel column chromatography (eluent: n-hexane--ethyl acetate=40:1) to obtain 29 g of ethyl 2-[4-(2,2-dichlorovinyl)phenyl]propionate (ST-5) as an oily substance, b.p.0.2-0.3 128°-129° C.

후처리

  1. temperatureAfter cooling
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customto give an oily substance, which

출처 및 근거

ORD 기록
ord-aba7aa42ef834a13bc5e27081e0e5eb7
출처 데이터셋
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04557871

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