Reaktion #5705

ord-60b3074aefe344eab4ea2ade849112af

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe cooling bath was removed
  2. 2
    workup.ADDITIONafter addition
  3. 3
    SonstigeThe precipitated white solid was collected
  4. 4
    Waschenwashed with ether-hexane (1:1)
  5. 5
    Sonstigerecrystallized from acetone-ethyl acetate-ether solvent mixture

Vorschrift

A magnetically stirred solution of methyl α-[3-(trifluoromethyl)benzylamino]-1-benzylindole-3-acetate (4.07 g, 9.0 mmol) in 65 mL of ether cooled at 0°-5° C. was treated dropwise over a four-minute period with a stock solution of hydrogen chloride in ether (3.8 mL, 11.71 mmol, 1.3 eq, 3.1 mmol per mL). The cooling bath was removed after addition was completed and the mixture stirred at room temperature overnight. The precipitated white solid was collected, washed with ether-hexane (1:1) and recrystallized from acetone-ethyl acetate-ether solvent mixture to yield 4.18 g (95%) of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05245046uspto-grants-1993_09