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Acetonitrile → 3-Cyclohexenylcarbonylacetonitrile

HRID 638646
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HRID 638646 반응식
[H-].[Na+].[CH:3]1([C:9]([O:11]CC)=O)[CH2:8][CH2:7][CH:6]=[CH:5][CH2:4]1.[C:14](#[N:16])[CH3:15]>C1(C)C=CC=CC=1>[CH:3]1([C:9]([CH2:15][C:14]#[N:16])=[O:11])[CH2:8][CH2:7][CH:6]=[CH:5][CH2:4]1
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참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 24758Sodium hydrideHCID 858033-Cyclohexene-1-carboxylic acid, ethyl ester

생성물 1

HCID 135375663-Cyclohexenylcarbonylacetonitrile수율 98.4%

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
85 °C

실험 절차

To a suspension of 1.25 g (2.60 mM) of 50% sodium hydride in 10 ml of toluene is added dropwise a solution of 2.01 g (1.30 mM) of ethyl 3-cyclohexenylcarboxylate 11 and 0.96 g (2.34 mM) of acetonitrile in 4 ml of toluene under nitrogen atmosphere in an hour and the mixture is stirred at 85° C. for 8 hours. After cooling, ice-cold water is added to the mixture. The aqueous phase is separated, washed with toluene, made acid with 10% hydrochloric acid and extracted with toluene. The extracted solution is washed with a dilute aqueous sodium hydrogencarbonate, and then with water, dried on magnesium sulfate and evaporated under reduced pressure. The resulting residue is chromatographed over silica gel and eluted with chloroform to give 1.91 g of the titled compound 8 as an yellow oil in 98.4% yield,

후처리

  1. temperatureAfter cooling
  2. additionice-cold water is added to the mixture
  3. customThe aqueous phase is separated
  4. washwashed with toluene
  5. extractionextracted with toluene
  6. washThe extracted solution is washed with a dilute aqueous sodium hydrogencarbonate
  7. dry with materialwith water, dried on magnesium sulfate
  8. customevaporated under reduced pressure
  9. customThe resulting residue is chromatographed over silica gel
  10. washeluted with chloroform

출처 및 근거

ORD 기록
ord-ae6faccf8e6a4ddd812766f993a6dc44
출처 데이터셋
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04562256

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