Imidazole → HCID 14626270, Verbindung

HRID 477783Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 477783
[OH:1][C:2]1[CH:17]=[CH:16][C:5]2[O:6][CH2:7][C:8]3[CH:15]=[CH:14][CH:13]=[CH:12][C:9]=3[C:10](=[O:11])[C:4]=2[CH:3]=1.N1C=CN=C1.[C:23]([Si:27]([CH3:30])([CH3:29])Cl)([CH3:26])([CH3:25])[CH3:24].C1(C)C=CC=CC=1>CN(C)C=O>[CH3:29][Si:27]([CH3:30])([C:23]([CH3:26])([CH3:25])[CH3:24])[O:1][C:2]1[CH:17]=[CH:16][C:5]2[O:6][CH2:7][C:8]3[CH:15]=[CH:14][CH:13]=[CH:12][C:9]=3[C:10](=[O:11])[C:4]=2[CH:3]=1

Komponenten

6

Edukt 4

HCID 795ImidazoleHCID 1140TolueneHCID 28928tert-Butyldimethylsilyl chlorideHCID 677495HCID 677495, Verbindung

Produkt 1

HCID 14626270HCID 14626270, VerbindungAusbeute 86,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 10 g of 2-hydroxy-6,11-dihydrodibenz[b,e]oxepin-11-one in 50 ml of dimethylformamide are added 6.5 g of imidazole and 7 g of t-butyldimethylchlorosilane and the mixture is stirred for 1 hour. After adding 300 ml of toluene, successively washing with water and a saturated saline solution and drying over magnesium sulfate, the solvent is distilled off under reduced pressure to give 13 g of 2-(dimethyl-t-butylsilyloxy)-6,11-dihydrodibenz[b,e]oxepin-11-one (oil). Mass spectrum m/z: 340(M+).

Aufarbeitung

  1. washsuccessively washing with water
  2. dry with materiala saturated saline solution and drying over magnesium sulfate
  3. distillationthe solvent is distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-bd69a7a676184ed994a6a2f6fee5647f
Quelldatensatz
uspto-grants-1989_12
Patentnummer
US04889858

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