Sodium sulfate decahydrate → (4-{[5-(4-fluorophenyl)-1-methyl-1H-pyrazol-4-yl]methoxy}phenyl)methanol

HRID 507922Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 507922
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([CH3:13])[N:11]=[CH:10][C:9]=2[CH2:14][O:15][C:16]2[CH:25]=[CH:24][C:19]([C:20](OC)=[O:21])=[CH:18][CH:17]=2)=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:12]([CH3:13])[N:11]=[CH:10][C:9]=2[CH2:14][O:15][C:16]2[CH:17]=[CH:18][C:19]([CH2:20][OH:21])=[CH:24][CH:25]=2)=[CH:6][CH:7]=1

Komponenten

5

Edukt 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 23157684methyl 4-{[5-(4-fluorophenyl)-1-methyl-1H-pyrazol-4-yl]methoxy}benzoate

Produkt 1

HCID 23157546(4-{[5-(4-fluorophenyl)-1-methyl-1H-pyrazol-4-yl]methoxy}phenyl)methanolAusbeute 80,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a solution of methyl 4-{[5-(4-fluorophenyl)-1-methyl-1H-pyrazol-4-yl]methoxy}benzoate (920 mg, 2.70 mmol) in tetrahydrofuran (10 mL) was added lithium aluminum hydride (200 mg, 5.27 mmol) at 0° C., and the mixture was stirred at 0° C. for 1 hr. Sodium sulfate decahydrate (1.0 g) was added to the reaction mixture, and the mixture was allowed to warm to room temperature and stirred for 30 min. The insoluble material was filtered off, and the filtrate was concentrated to give the title compound (680 mg, yield 80%) as a yellow oil.

Aufarbeitung

  1. temperatureto warm to room temperature
  2. stirringstirred for 30 min
  3. filtrationThe insoluble material was filtered off
  4. concentrationthe filtrate was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-c7ba7f0a46724657a2d484d6b7752823
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07786165B2

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