Reaktion #1333383

ord-e458f7df25e24ceaa55590b29ab7f43d

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeHCl was bubbled into the solution for 50 minutes until the mixture
  2. 2
    SonstigeThe ether was decanted off
  3. 3
    workup.DISSOLUTIONdissolved in methanol
  4. 4
    EinengenThe methanol solution was concentrated in vacuum

Vorschrift

A solution of intermediate (19) (0.004 mole) and HCl/diethylether (60 mL) was cooled in an ice bath under argon. Ethanol (0.0075 mole) was added. HCl was bubbled into the solution for 50 minutes until the mixture became homogeneous. The mixture was allowed to slowly warm to room temperature and stir for 4 hours. The ether was decanted off and dissolved in methanol. The methanol solution was concentrated in vacuum and the residue was used as is for the next step, yielding ethyl 1-acetyl-5-fluoro-2,3-dihydro-1H-indole-2-carboximidate monohydrochloride (intermediate 20).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07125891B2uspto-grants-2006_10