Reaktion #168912

ord-da557bd64a7e4ba493a12453796b8043

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationIt was filtered
  2. 2
    Sonstigeto remove any inorganic material
  3. 3
    Einengenthe dimethyl formamide solution was concentrated in vacuo
  4. 4
    Sonstigechromatographed on the silica gel

Vorschrift

To a stirred mixture of 4-(3-(bromomethyl)phenylthio)-N-(4-morpholinophenyl)pyrimidin-2-amine (100 mg, 0.22 mmol) and 4-cyanomethyl imidazole (47 mg, 0.44 mmol) in dimethyl formamide (2 mL), was added cesium carbonate (154 mg, 0.44 mmol) in one portion. The mixture was stirred at room temperature for 16 hours. It was filtered to remove any inorganic material, and the dimethyl formamide solution was concentrated in vacuo. The residue was column chromatographed on the silica gel using methanol:dichloromethane (4:96) as eluant to give the product (50 mg, 47%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846704B2uspto-grants-2014_09