StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Aluminium lithium hydride → HCID 12277043, Verbindung

HRID 2408244
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2408244
[CH3:1]/[C:2](=[CH:9]\[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)/[CH2:3][CH2:4][C:5](OC)=[O:6].[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[CH3:1]/[C:2](=[CH:9]\[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)/[CH2:3][CH2:4][CH2:5][OH:6]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 21226445Aluminium lithium hydrideHCID 67330102HCID 67330102, Verbindung

Produkt 1

HCID 12277043HCID 12277043, VerbindungAusbeute 102,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of methyl (4E)-4-methyl-5-phenyl-4-pentenoate (3.5 g, 0.016 mol) in dry THF (100 ml) was treated, at −78° C. under nitrogen, with solid lithium aluminum hydride (1 g, 0.025 mol) in one portion. After 5 minutes, the cooling bath was removed and the reaction allowed reaching room temperature and then cooled to 0° C. and treated successively with water (1 ml), 5% aqueous sodium hydroxide (3 ml) and water (1 ml). The reaction was stirred at room temperature for 30 minutes. Anhydrous solid sodium sulfate was added (3 g) and stirring continued for 5 minutes. The solid was filtered off, rinsed with diethyl ether and the filtrate was evaporated under vacuum. The product was purified by bulb-to-bulb distillation (84° C./0.002 mbar). 2.88 g (yield=100%) of the desired product were obtained.

Aufarbeitung

  1. customthe cooling bath was removed
  2. customallowed reaching room temperature
  3. additiontreated successively with water (1 ml), 5% aqueous sodium hydroxide (3 ml) and water (1 ml)
  4. additionAnhydrous solid sodium sulfate was added (3 g)
  5. stirringstirring
  6. waitcontinued for 5 minutes
  7. filtrationThe solid was filtered off
  8. washrinsed with diethyl ether
  9. customthe filtrate was evaporated under vacuum
  10. distillationThe product was purified by bulb-to-bulb distillation (84° C./0.002 mbar)

Quellen und Nachweise

ORD-Eintrag
ord-da87a77f9e2d4c939576883b130145ba
Quelldatensatz
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08815792B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion