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Hydrogen Peroxide → HCID 10989376, Verbindung

HRID 2257430
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2257430
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]#[C:10][C:11]2[CH:16]=[CH:15][C:14](Br)=[CH:13][CH:12]=2)=[CH:5][CH:4]=1)#[N:2].CN1[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1.C(=O)([O-])[O-].[K+].[K+].[OH-].[Na+].OO>O1CCCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]#[C:10][C:11]2[CH:16]=[CH:15][C:14](/[CH:20]=[CH:21]/[CH2:22][CH2:23][CH3:24])=[CH:13][CH:12]=2)=[CH:5][CH:4]=1)#[N:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 784Hydrogen PeroxideHCID 11430Potassium CarbonateHCID 12291N-MethylpiperidineHCID 14798Sodium HydroxideHCID 229228794-[(4-Bromophenyl)ethynyl]benzonitrile

Produkt 1

HCID 10989376HCID 10989376, VerbindungAusbeute 84 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418397HCID 178418397, VerbindungKatalysatorHCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

In a four necked flask equipped with a stirrer, a reflux condenser and a thermometer which had been replaced by a nitrogen atmosphere, 1-(4-cyanophenyl)-2-(4-bromophenyl)acetylene (3.4 g, 12 mmol), tetrakis(triphenylphosphine)palladium (0.23 g, 0.2 mmol), N-methylpiperidine (5 g), potassium carbonate (5.5 g, 40 mmol) and tetrahydrofuran (60 ml) were charged. Then, to the mixture, a solution of E-1-pentenylcatecholborane (20 mmol) in tetrahydrofuran (50 ml) was dropwise added at room temperature, followed by heat refluxing for 6 hours while stirring. After cooling the reaction mixture to room temperature, 10% aqueous solution of sodium hydroxide (5 ml) and 30% aqueous hydrogen peroxide (2 ml) were added to the mixture, followed by stirring for 1 hour. The mixture was extracted with ethyl ether. The organic layer was washed with saturated aqueous solution of sodium chloride (20 ml each) twice and dried over anhydrous magnesium sulfate. After evaporating the solvent off, the residue was purified by silica gel column chromatography to obtain 1-(4-cyanophenyl)-2-[4-(1-trans-pentenyl)phenyl]acetylene (2.7 g). Yield: 84%.

Aufarbeitung

  1. customIn a four necked flask equipped with a stirrer, a reflux condenser
  2. additionwere charged
  3. temperatureby heat
  4. temperaturerefluxing for 6 hours
  5. stirringby stirring for 1 hour
  6. extractionThe mixture was extracted with ethyl ether
  7. washThe organic layer was washed with saturated aqueous solution of sodium chloride (20 ml each) twice
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customAfter evaporating the solvent off, the residue
  10. customwas purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-aa6d3758769d4f76899b3b54367f78ec
Quelldatensatz
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05658489

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