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Triphenylphosphine → HCID 53960761, Verbindung

HRID 1379916
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1379916
[CH3:1][C@@H:2]([CH2:6][CH2:7][CH:8](O)[C:9]([CH3:11])=[CH2:10])[CH2:3][CH2:4][OH:5].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH3:1][C@@H:2]([CH2:6][CH:7]=[CH:8][C:9]([CH3:11])=[CH2:10])[CH2:3][CH2:4][OH:5]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 11776TriphenylphosphineHCID 86751364HCID 86751364, Verbindung

Produkt 1

HCID 53960761HCID 53960761, VerbindungAusbeute 80,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 167845palladium(II) acetateKatalysator

Versuchsvorschrift

(S)-3,7-dimethyl-6-hydroxy-7-octene-1-ol (I) (10.0 g, 58.1 mmol), palladium acetate (130.0 mg, 0.579 mmol), and triphenylphosphine (1.52 g, 5.795 mmol) were placed in a 50 ml three neck distillation flask provided with a thermometer and a vacuum distilling apparatus having a side arm. Butanol (20 ml) was then added to the flask and the mixture was heated for 12 hours with stirring at a reaction temperature of 115° to 120° C. and a atmospheric pressure in a stream of nitrogen. After the reaction had terminated, the flask was evacuated to remove solvent from the reaction mixture, and the resultant was distilled to obtain 7.2 g (89° to 91° C./4 mmHg) of (S)-3,7-dimethyl-5,7-octadiene-1-ol (II). The yield was 80%.

Aufarbeitung

  1. customprovided with a thermometer
  2. distillationa vacuum distilling apparatus
  3. additionButanol (20 ml) was then added to the flask
  4. temperaturethe mixture was heated for 12 hours
  5. customAfter the reaction had terminated
  6. customthe flask was evacuated
  7. customto remove solvent from the reaction mixture
  8. distillationthe resultant was distilled

Quellen und Nachweise

ORD-Eintrag
ord-4d8bca6730c948cc8bea4c883a82c1c7
Quelldatensatz
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05672783

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