Reaktion #527657

ord-bd1943f6d7964225824729a2f255c1f1

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe solvent removed by evaporation
  2. 2
    workup.ADDITIONWater was added
  3. 3
    Extraktionthe mixture extracted with ether

Vorschrift

A solution of methyl iodide (1.9 g) in acetone (20 ml) was added dropwise to a stirred suspension of 1-[1-(2,4-dichlorophenyl)cyclobutyl]-6,7-dimethoxy-1,2,3,4-tetrahydroisoquinoline (4 g prepared as described in Example RC9) and anhydrous potassium carbonate (3.1 g) in acetone (70 ml). The mixture was stirred at ambient temperature for 90 minutes and the solvent removed by evaporation. Water was added and the mixture extracted with ether. The ether layer yielded 1-[1-(2,4-dichlorophenyl)cyclobutyl]-6,7-dimethoxy-2-methyl-1,2,3,4-tetrahydroisoquinoline as an oil. A portion of this oil was characterised by conversion into its 1.5 oxalate salt, m.p. 125°-132° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05519034uspto-grants-1996_05