Aluminium lithium hydride → HCID 20031090, Verbindung

HRID 232149Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 232149
C([O:3][C:4]([C:6]1[C:10]2[CH2:11][CH2:12][CH2:13][C:9]=2[N:8]([CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[N:7]=1)=O)C.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[CH2:14]([N:8]1[C:9]2[CH2:13][CH2:12][CH2:11][C:10]=2[C:6]([CH2:4][OH:3])=[N:7]1)[C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

Komponenten

4

Edukt 2

HCID 21226445Aluminium lithium hydrideHCID 54375111HCID 54375111, Verbindung

Produkt 1

HCID 20031090HCID 20031090, VerbindungAusbeute 1.065,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A solution of 1-benzyl-1,4,5,6-tetrahydro-3-cyclopentapyrazole carboxylic acid ethyl ester (6.0 g, 2.22 mmol) in THF (125 ml) was treated with lithium aluminum hydride (1.73 g, 44.4 mmol) and reacted at ambient temperature for 3.5 hours. Excess reagent was quenched with 10% aqueous THF (18 ml), 15% sodium hydroxide (5.4 ml) and water (5.4 ml). The mixture was diluted with ethyl acetate and filtered. The filtrate was washed with 5% brine solutions, dried, and evaporated to provide the title compound (5.40 g) as an oil.

Aufarbeitung

  1. customreacted at ambient temperature for 3.5 hours
  2. customExcess reagent was quenched with 10% aqueous THF (18 ml), 15% sodium hydroxide (5.4 ml) and water (5.4 ml)
  3. additionThe mixture was diluted with ethyl acetate
  4. filtrationfiltered
  5. washThe filtrate was washed with 5% brine solutions
  6. customdried
  7. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-ba1834a51b864f498493990d2345a5a1
Quelldatensatz
uspto-grants-1989_07
Patentnummer
US04851425

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