Reaktion #1528399

ord-167148461f49402e8f84650cda7d4398

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigewas evaporated
  2. 2
    workup.DISSOLUTIONthe residue dissolved in dimethoxy ethane (25 ml)
  3. 3
    workup.ADDITIONDBU (1,8-diazabicyclo[5.4.0]undec-7-en) was added (1.78 g)
  4. 4
    Temperaturthe reaction mixture heated
  5. 5
    Temperaturunder reflux for 1 hour

Vorschrift

A solution of 2-(4-fluoro-phenyl)-1-phenyl-ethylamine (1.50 g) in THF was treated dropwise with 2-chloroethyl isocyanate (0.89 g) at 0° C. After stirring overnight at room temperature the solvent was evaporated and the residue dissolved in dimethoxy ethane (25 ml). DBU (1,8-diazabicyclo[5.4.0]undec-7-en) was added (1.78 g) and the reaction mixture heated under reflux for 1 hour. Column chromatography on silica yielded 1.3 g of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07655600B2uspto-grants-2010_02