Aluminium lithium hydride → HCID 63322063, Verbindung

HRID 32460

Reaktionsgleichung

Reaktionsgleichung von HRID 32460
[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10](=O)[CH2:11][CH2:12][C:13]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[N:14]O)[CH2:6][CH2:5]1)([CH3:3])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([CH2:10][CH2:11][CH2:12][CH:13]([NH2:14])[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:6][CH2:5]1)([CH3:3])[CH3:2]

Komponenten

4

Edukt 2

HCID 21226445Aluminium lithium hydrideHCID 866036021-(4-Isopropylpiperazin-1-yl)-4-phenylbutane-1,4-dione 4-oxime

Produkt 1

HCID 63322063HCID 63322063, VerbindungAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

To a solution of 1-(4-isopropylpiperazin-1-yl)-4-phenylbutane-1,4-dione 4-oxime (625 mg, 2.0 mmol) in 10 mL of THF was slowly added lithium aluminum hydride (250 mg, 6.6 mmol). The reaction flask was heated at 70° C. for 4 h after which time the flask was cooled to 0 C and the reaction was quenched by slow addition of water and 1 N sodium hydroxide. The biphasic mixture was filtered through a pad of diatomaceous earth, and the filtered solution was concentrated to dryness to afford 536 mg (98%) of the title compound as a crude residue that was used without further purification.

Aufarbeitung

  1. temperaturewas cooled to 0 C
  2. customthe reaction was quenched by slow addition of water and 1 N sodium hydroxide
  3. filtrationThe biphasic mixture was filtered through a pad of diatomaceous earth
  4. concentrationthe filtered solution was concentrated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-fd4558891c2746bcb49800b4bddd4e77
Quelldatensatz
uspto-grants-2008_09
Patentnummer
US07427632B2

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