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Aluminium lithium hydride → HCID 59403541, Verbindung

HRID 1514195
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1514195
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([CH2:13][O:14][C:15]2[CH:26]=[CH:25][C:18]3[C:19](=O)[NH:20][CH2:21][CH2:22][O:23][C:17]=3[CH:16]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C1COCC1>[C:7]1([CH2:13][O:14][C:15]2[CH:26]=[CH:25][C:18]3[CH2:19][NH:20][CH2:21][CH2:22][O:23][C:17]=3[CH:16]=2)[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 21226445Aluminium lithium hydrideHCID 59403479HCID 59403479, Verbindung

Produkt 1

HCID 59403541HCID 59403541, VerbindungAusbeute 94,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

1M Lithium aluminium hydride (62.4 ml, 62.4 mmol) in THF was added under argon to a stirred solution of 8-[(phenylmethyl)oxy]-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (Preparation 27) (8.39 g, 31.2 mmol) in THF (150 ml) with ice bath cooling over 5 minutes. The resulting solution was heated with stirring at 60° C. for 3 hours. The reaction was cooled and carefully quenched by slow addition with ice cooling of 150 ml of 2M sodium hydroxide followed by 150 ml of EtOAc. The organics were separated and aqueous extracted with 100 ml of EtOAc. The combined organic extracts were dried (magnesium sulphate) and evaporated to give the title compound (7.53 g) as a light coloured oil. MS (ES) C16H17NO2 requires 255; found 256 [M+H]+.

Aufarbeitung

  1. temperaturecooling over 5 minutes
  2. temperatureThe resulting solution was heated
  3. temperatureThe reaction was cooled
  4. customcarefully quenched by slow addition with ice
  5. temperaturecooling of 150 ml of 2M sodium hydroxide
  6. customThe organics were separated
  7. extractionaqueous extracted with 100 ml of EtOAc
  8. dry with materialThe combined organic extracts were dried (magnesium sulphate)
  9. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-d7072acb7be646208263080ab6a7f676
Quelldatensatz
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08222245B2

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