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Hydrochloric Acid → HCID 11321150, Verbindung

HRID 1655764
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1655764
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([C@H:13]([CH:17]([CH3:19])[CH3:18])[C:14](O)=[O:15])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.Cl>CCOCC>[C:7]1([C@H:13]([CH:17]([CH3:19])[CH3:18])[CH2:14][OH:15])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 7233172(S)-3-methyl-2-phenylbutanoic acidHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 11321150HCID 11321150, VerbindungAusbeute 105,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

A suspension of 19.5, g (0.51 mol) of lithium aluminium hydride in 750 ml of absolute ether was heated to reflux. Within 4 hours there was added, dropwise, a solution of 54.5 g (0.307 mol) of (S)-(+)-2-phenyl 3-methylbutyric acid in 250 ml of absolute ether. After heating to reflux for a further 2 hours, the suspension was treated carefully with 1N hydrochloric acid and the ether phase was washed with water, dilute sodium bicarbonate solution, and once more with water. After drying the organic phase over sodium sulfate and evaporation under reduced pressure, there were obtained 53.1 g of (S)-(+)-2-phenyl-3-methylbutanol as a thick oil which was used directly in the next step.

Aufarbeitung

  1. temperaturewas heated to reflux
  2. additionWithin 4 hours there was added
  3. temperatureAfter heating
  4. temperatureto reflux for a further 2 hours
  5. washthe ether phase was washed with water, dilute sodium bicarbonate solution
  6. customAfter drying the organic phase
  7. customover sodium sulfate and evaporation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-03e11201694046bcbabb459347e33315
Quelldatensatz
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05250517

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