Reaktion #1543732

ord-dc7b980efa9f477b9076448de9cd7e78

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenthe solution was concentrated by evaporation under reduced pressure
  2. 2
    workup.DISSOLUTIONThe resulting oily substance was dissolved in 5 ml of ethyl acetate
  3. 3
    SonstigeThe crystals which precipitated
  4. 4
    Filtrationwere collected by filtration
  5. 5
    Sonstigedried in vacuo

Vorschrift

138 mg of (2R,4R)-2-[2-{4-fluoro-2-[2-(4-fluorophenyl)ethyl]phenoxy}ethyl]-4-hydroxy-1-methylpyrrolidine [prepared as described in step (b) above] were dissolved in 4 ml of ethyl acetate, and then 0.15 ml of a 4N solution of hydrogen chloride in ethyl acetate was added to the resulting solution, and the solution was concentrated by evaporation under reduced pressure. The resulting oily substance was dissolved in 5 ml of ethyl acetate, and the resulting solution was allowed to stand at room temperature for about 10 minutes. The crystals which precipitated were collected by filtration, and dried in vacuo, to give 66 mg (yield 43%) of the title compound as colorless crystals, melting at 70°-73° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05843983uspto-grants-1998_12