Reaktion #317459

ord-9b1c54c983684c15839ffc481646e339

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent is removed in vacuo
  2. 2
    Sonstigethe product is purified via preparative HPLC (RP18-column; eluent: acetonitrile-water, gradient 10:90 to 90:10)

Vorschrift

Ethyl 4-(4-cyanophenyl)-6-methyl-2-thioxo-1-[3-(trifluoromethyl)phenyl]-1,2,3,4-tetrahydro-5-pyrimidinecarboxylate (Example 3; 100 mg, 0.22 mmol), 4-(bromo-methyl)pyridine hydrobromide (62.5 mg, 0.25 mmol), N,N,N-tributyl-1-butan-aminium iodide (7 mg, 0.03 mmol) and potassium carbonate (65.2 mg, 0.47 mmol) are dissolved in 3 ml acetone and stirred at room temperature overnight. The solvent is removed in vacuo and the product is purified via preparative HPLC (RP18-column; eluent: acetonitrile-water, gradient 10:90 to 90:10).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07566723B2uspto-grants-2009_07