Reaktion #1594973

ord-633b93ad28744eda8b8fecc692e0cca1

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with ethyl acetate, brine
  2. 2
    Trocknendried over Na2SO4
  3. 3
    SonstigeAfter removing the solvents under reduced pressure
  4. 4
    Sonstigethe residue was purified by chromatography on silica gel (hexane/EtOAc 5:1)

Vorschrift

To a solution of 2-(4-fluorobenzyl)-7-(methylthio)thiazolo[5,4-d]pyrimidin-5-amine (0.4 g, 1.31 mmol) and 2N NaOH (0.65 ml, 1.31 mmol) in DMSO (7 ml) was added iodomethane (81 μl, 1.31 mmol). The reaction mixture was stirred at room temperature for 2 hours. The mixture was poured into water and extracted with ethyl acetate, brine and dried over Na2SO4. After removing the solvents under reduced pressure, the residue was purified by chromatography on silica gel (hexane/EtOAc 5:1) yielding the title compound as a white solid (0.29 g, 69%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09221822B2uspto-grants-2015_12