10-Methoxyiminostilbene → 10-methoxy-5H-dibenz(b,f)azepine-5-carboxamide

HRID 2373529

Reaktionsgleichung

Reaktionsgleichung von HRID 2373529
[CH3:1][O:2][C:3]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[NH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=1.[O-:18][C:19]#[N:20].[Na+].C(O)(=O)/C=C\C(O)=O>ClCCl>[CH3:1][O:2][C:3]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:11]([C:19]([NH2:20])=[O:18])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=1

Komponenten

5

Edukt 3

HCID 7842410-MethoxyiminostilbeneHCID 444266Maleic AcidHCID 517096Sodium Cyanate

Produkt 1

HCID 12003110-methoxy-5H-dibenz(b,f)azepine-5-carboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a 1 L 4-necked round bottom flask was added 10.0 g (0.045 mol) of 10-methoxyiminostilbene, 150.0 ml of dichloromethane, 37.0 g (0.57 mol) of sodium cyanate and 15.0 g (0.13 moles) of maleic acid and stirred at room temperature. The contents were heated to reflux (40-45° C.) under vigorous stirring for about 6 to about 8 hours. After completion of the reaction (detected by TLC) the reaction mass was filtered and washed with 50.0 ml dichloromethane. The dichloromethane layer was washed with water (50.0 ml×2) and the layers were separated.

Aufarbeitung

  1. temperatureThe contents were heated
  2. temperatureto reflux (40-45° C.)
  3. stirringunder vigorous stirring for about 6 to about 8 hours
  4. customAfter completion of the reaction (detected by TLC) the reaction mass
  5. filtrationwas filtered
  6. washwashed with 50.0 ml dichloromethane
  7. washThe dichloromethane layer was washed with water (50.0 ml×2)
  8. customthe layers were separated

Quellen und Nachweise

ORD-Eintrag
ord-85a333037c23477695f1d21a68f04e93
Quelldatensatz
uspto-grants-2008_12
Patentnummer
US07459553B2

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