Benzyl Chloride → 1-Benzyl-hexahydro-7-phenyl-1,4-diazepin-5-one

HRID 1637167Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1637167
[C:1]1([CH:7]2[NH:13][CH2:12][CH2:11][NH:10][C:9](=[O:14])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:21](Cl)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>C(#N)C>[CH2:21]([N:13]1[CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH2:8][C:9](=[O:14])[NH:10][CH2:11][CH2:12]1)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1

Komponenten

5

Edukt 3

HCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 130482357-Phenyl-1,4-diazepan-5-one

Produkt 1

HCID 193479331-Benzyl-hexahydro-7-phenyl-1,4-diazepin-5-oneAusbeute 83,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

1.9 g hexahydro-7-phenyl-1,4-diazepin-5-one (for preparation see Example 1C) in 30 ml acetonitrile were heated to boiling with 2.0 g potassium carbonate and 1.2 g benzyl chloride with reflux cooling for 36 hours. Then filtration was carried out and the filtrate reduced in volume. The remaining residue was shaken with 10% aqueous citric acid solution, the organic phase was separated, dried over magnesium sulfate and reduced in volume under a vacuum. 2.23 g crude 1-benzyl-hexahydro-7-phenyl-1,4-diazepin-5-one were obtained as an oil, which was used for the next synthesis stage without further purification or characterization.

Aufarbeitung

  1. temperaturewith reflux
  2. temperaturecooling for 36 hours
  3. filtrationThen filtration
  4. customthe organic phase was separated
  5. dry with materialdried over magnesium sulfate

Quellen und Nachweise

ORD-Eintrag
ord-6d0163b8cb4649f29ae48e11f811ce12
Quelldatensatz
uspto-grants-2000_03
Patentnummer
US06040303

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