Reaktion #604426

ord-0373ef94d1eb4504b9e7d77f3580ccf0

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigepurified by reversed phase HPLC (Waters Xbridge™-C18, gradient of acetonitrile in water, 0.1% NH3)
  2. 2
    Sonstige0.91 min (Z011_S03)

Vorschrift

Potassium carbonate (67 mg, 0.486 mmol) is added to a solution of 4-(2,5-dioxo-1-(3-(tri-fluoromethyl)phenyl)-1,2,3,4,5,6,7,8-octahydroquinazolin-4-yl)-benzonitrile (example 1, 100 mg, 0.243 mmol) in N,N-dimethylformamide (3 mL). 3-(Bromomethyl)tetrahydrofuran (60 mg, 0.365 mmol) is added, and the mixture is stirred at room temperature for 1 h and purified by reversed phase HPLC (Waters Xbridge™-C18, gradient of acetonitrile in water, 0.1% NH3). Yield: 12 mg; ESI mass spectrum [M+H]+=496; Retention time HPLC: 0.91 min (Z011_S03).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09115093B2uspto-grants-2015_08