Sodium sulfate decahydrate → 3-Ethoxy-5-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyl alcohol

HRID 1295215Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1295215
C([O:3][C:4](=O)[C:5]1[CH:10]=[C:9]([O:11][CH2:12][C:13]2[N:14]=[C:15]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[O:16][C:17]=2[CH3:18])[CH:8]=[C:7]([O:25][CH2:26][CH3:27])[CH:6]=1)C.[H-].[Li+].[Al+3].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.[O-]S([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH2:26]([O:25][C:7]1[CH:6]=[C:5]([CH:10]=[C:9]([O:11][CH2:12][C:13]2[N:14]=[C:15]([C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=3)[O:16][C:17]=2[CH3:18])[CH:8]=1)[CH2:4][OH:3])[CH3:27]

Komponenten

5

Edukt 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 22930682Ethyl 3-ethoxy-5-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzoate

Produkt 1

HCID 694273333-Ethoxy-5-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyl alcoholAusbeute 92,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of ethyl-3-ethoxy-5-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzoate (5.40 g) in tetrahydrofuran (80 ml) was gradually added aluminum lithium hydride (540 mg) at 0° C. and the mixture was stirred for 1 hr. Sodium sulfate 10 hydrate (4.60 g) was added to the reaction mixture and the mixture was further stirred for 30 min. The insoluble materials were filtered off, and the filtrate was concentrated. The obtained crystals were recrystallized from ethyl acetate-isopropyl ether to give 3-ethoxy-5-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyl alcohol (4.44 g, 92%) as colorless needle-shaped crystals. melting point: 103–104° C.

Aufarbeitung

  1. customat 0° C.
  2. stirringthe mixture was further stirred for 30 min
  3. filtrationThe insoluble materials were filtered off
  4. concentrationthe filtrate was concentrated
  5. customThe obtained crystals were recrystallized from ethyl acetate-isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-b2c65d1d1220496bb4a50abd327355f0
Quelldatensatz
uspto-grants-2007_07
Patentnummer
US07241785B2

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