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Water → 4-[2-(p-Pentylphenyl)ethenyl]cyclohexanecarbonitrile

HRID 370369
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 370369
[Br-].[CH2:2]([C:7]1[CH:32]=[CH:31][C:10]([CH2:11][P+](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=[CH:9][CH:8]=1)[CH2:3][CH2:4][CH2:5][CH3:6].[C:33]([CH:35]1[CH2:40][CH2:39][CH:38]([CH:41]=O)[CH2:37][CH2:36]1)#[N:34].O>COC(C)(C)C>[CH2:2]([C:7]1[CH:32]=[CH:31][C:10]([CH:11]=[CH:41][CH:38]2[CH2:39][CH2:40][CH:35]([C:33]#[N:34])[CH2:36][CH2:37]2)=[CH:9][CH:8]=1)[CH2:3][CH2:4][CH2:5][CH3:6]
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Komponenten

5

Edukt 3

HCID 962WaterHCID 13548132trans-4-FormylcyclohexanecarbonitrileHCID 21285310p-Pentylbenzyl-triphenylphosphonium bromide

Produkt 1

HCID 542178694-[2-(p-Pentylphenyl)ethenyl]cyclohexanecarbonitrileAusbeute 81 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 15413tert-Butyl methyl etherLösungsmittel

Versuchsvorschrift

A mixture of 2.51 g of p-pentylbenzyl-triphenylphosphonium bromide and 615 mg of a cis/trans mixture (about 1:1) of 4-cyanocyclohexanecarboxaldehyde in 30 ml of t-butyl methyl ether was placed at 0° C. under argon gasification in a sulphonation flask fitted with a thermometer and solid substance addition tube, treated within 2 minutes with 673 mg of solid potassium t-butylate and subsequently stirred for a further 1.5 hours. The red-brown heterogeneous mixture was then poured into 100 ml of water and extracted three times with 100 ml of diethyl ether each time. The organic phases were washed twice with 50 ml of water each time and once with 50 ml of saturated sodium chloride solution, dried over magnesium sulphate and concentrated. The residue was suspended in 150 ml of hexane, freed from precipitated triphenylphosphine oxide by filtration (rinsing with hexane) and the filtrate was concentrated. Low-pressure chromatography (0.4 bar) of the resulting oil (1.36 g) on silica gel using 3% ethyl acetate/petroleum ether as the eluting agent gave 1.02 g (81%) of 4-[2-(p-pentylphenyl)ethenyl]cyclohexanecarbonitrile as a colourless oil; Rf values (10% ethyl acetate/petroleum ether): 0.27 and 0.37 (stereoisomer mixture).

Aufarbeitung

  1. customwas placed at 0° C. under argon
  2. customfitted with a thermometer and solid substance addition tube
  3. extractionextracted three times with 100 ml of diethyl ether each time
  4. washThe organic phases were washed twice with 50 ml of water each time
  5. dry with materialonce with 50 ml of saturated sodium chloride solution, dried over magnesium sulphate
  6. concentrationconcentrated
  7. customfrom precipitated triphenylphosphine oxide
  8. filtrationby filtration (rinsing with hexane)
  9. concentrationthe filtrate was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-79739dd00f2c4e798e0008762c98e571
Quelldatensatz
uspto-grants-1985_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04526704

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