Sodium sulfate decahydrate → 2-(5-Methyl-2-phenyl-4-oxazolylmethoxy)-4-pyridylmethanol

HRID 349948Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 349948
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]1[O:12][C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[N:10][C:9]=1[CH2:19][O:20][C:21]1[CH:26]=[C:25]([C:27](OC)=[O:28])[CH:24]=[CH:23][N:22]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:7][C:8]1[O:12][C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[N:10][C:9]=1[CH2:19][O:20][C:21]1[CH:26]=[C:25]([CH2:27][OH:28])[CH:24]=[CH:23][N:22]=1

Komponenten

5

Edukt 3

HCID 62649Sodium sulfate decahydrateHCID 17861336Methyl 2-(5-methyl-2-phenyl-4-oxazolyl)methoxy-4-pyridinecarboxylateHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 178613752-(5-Methyl-2-phenyl-4-oxazolylmethoxy)-4-pyridylmethanolAusbeute 77 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Lithium aluminium hydride (228 mg) was added to a solution of methyl 2-(5-methyl-2-phenyl-4-oxazolylmethoxy)-4-pyridinecarboxylate (1.95 g) in tetrahydrofuran (20 ml) at 0° C., which was stirred at room temperature for 30 minutes. Sodium sulfate decahydrate (1.93 g) was added to the reaction mixture, which was stirred at room temperature for 30 minutes. The precipitates were removed by filtration, the filtrate was concentrated. The resulting colorless crystals were collected by filtration to obtain 2-(5-methyl-2-phenyl-4-oxazolylmethoxy)-4-pyridylmethanol (1.37 g, yield 77%). This was recrystallized from ethyl acetate-hexane. Melting point: 100–101° C.

Aufarbeitung

  1. stirringwas stirred at room temperature for 30 minutes
  2. customThe precipitates were removed by filtration
  3. concentrationthe filtrate was concentrated
  4. filtrationThe resulting colorless crystals were collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-1e87c65db03f4f78831acb664f1c0722
Quelldatensatz
uspto-grants-2007_02
Patentnummer
US07179823B1

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