Reaktion #499790

ord-edc995e474914abeab1f7dda054d6543

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter completion of the reaction
  2. 2
    Sonstigethe solvent was evaporated
  3. 3
    workup.ADDITIONwater was added
  4. 4
    ExtraktionThe mixture was extracted with chloroform
  5. 5
    Trocknenthe organic layer was dried over anhydrous sodium sulfate
  6. 6
    SonstigeThe solvent was evaporated
  7. 7
    Sonstigethe obtained residue was purified by silica gel column chromatography (chloroform:methanol=4:1)
  8. 8
    Sonstigedried under reduced pressure

Vorschrift

To 4-aminomethyl-1-(pyridin-4-yl)piperidine-4-carboxylic acid ethyl ester dihydrobromide (423 mg) were added pyridine (2 ml) and 7-chlorosulfonyl-2-trifluoroacetyl-1,2,3,4-tetrahydroisoquinoline (273 mg), and the mixture was stirred at room temperature for 2 hours. After completion of the reaction, the solvent was evaporated and water was added. The mixture was extracted with chloroform and the organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated and the obtained residue was purified by silica gel column chromatography (chloroform:methanol=4:1) and dried under reduced pressure to give the title compound (222 mg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06562828B1uspto-grants-2003_05