Sodium Sulfate → 3,5-Dimethyl-4-(hydroxymethyl)isoxazole

HRID 359822

Reaktionsgleichung

Reaktionsgleichung von HRID 359822
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([C:12]1[C:13]([CH3:18])=[N:14][O:15][C:16]=1[CH3:17])(OCC)=[O:8].S([O-])([O-])(=O)=O.[Na+].[Na+]>CCOCC>[CH3:18][C:13]1[C:12]([CH2:7][OH:8])=[C:16]([CH3:17])[O:15][N:14]=1

Komponenten

5

Edukt 3

HCID 24436Sodium SulfateHCID 736348Ethyl 3,5-dimethylisoxazole-4-carboxylateHCID 21226445Aluminium lithium hydride2×

Produkt 1

HCID 2895753,5-Dimethyl-4-(hydroxymethyl)isoxazoleAusbeute 75,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

To a suspension of 23.53 g of lithium aluminum hydride in 600 ml of ether was added dropwise 64 g of 4-carbethoxy-3,5-dimethylisoxazole in 100 ml of ether at a rate so that gentle reflux occurred. The addition was complete in about two hours, and the mixture was stirred overnight under nitrogen. A saturated solution of sodium sulfate was added dropwise under nitrogen until the excess lithium aluminum hydride was decomposed. The resulting suspension was filtered and the filtrate concentrated to an oil which was distilled to give 36.4 g of 3,5-dimethyl-4-hydroxymethylisoxazole, b.p. 130°-140° C. (0.1 mm).

Aufarbeitung

  1. temperaturethat gentle reflux
  2. additionThe addition
  3. filtrationThe resulting suspension was filtered
  4. concentrationthe filtrate concentrated to an oil which
  5. distillationwas distilled

Quellen und Nachweise

ORD-Eintrag
ord-216dd9ccd641402aab34f64cd3767c27
Quelldatensatz
uspto-grants-1991_03
Patentnummer
US05002960

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