Reaktion #1838261

ord-f4bff5cb06fe45518b6c7cb4ebb8e57a

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with water and brine
  2. 2
    Trocknendried (MgSO4)
  3. 3
    Sonstigeevaporated
  4. 4
    SonstigeThe residue was purified by PTLC (5% methanol/dichloromethane)

Vorschrift

tert-Butyl 3-((1-cyclohexyl-4-oxo-1,3,8-triazaspiro[4.5]decan-3-yl)methyl)benzoate (0.353 g, 0.826 mmol), 4-iodo-4′-fluorobutyrophenone (0.27 g, 0.826 mmol), and potassium carbonate (0.17 g, 1.24 mmol) in N,N-dimethylformamide (8 mL) were heated at 65° C. for 2 hours. The reaction was diluted with ethyl acetate, washed with water and brine, dried (MgSO4), and evaporated. The residue was purified by PTLC (5% methanol/dichloromethane) to give product as an oil (0.39 g, 80%); MS for C35H46FN3O4 m/z 592 (M+H)+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09156840B2uspto-grants-2015_10