Reaktion #486230

ord-92668cfc88624526a78b8d81ee6f057e

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGThis solution was then stirred at room temperature for 18 h
  2. 2
    Sonstigethe volatiles were evaporated
  3. 3
    workup.ADDITIONthe residue was diluted with water
  4. 4
    ExtraktionExtraction with ethyl acetate

Vorschrift

To a solution of 1H-indazole-3-carboxylic acid (0.745 g, 4.6 mmol) in 20 mL dimethylformamide, was added 1,1'-carbonyldiimidazole (0.745 g, 4.6 mmol). This mixture was stirred at room temperature for 4 h, and to it was added dropwise a solution of 1-(4-aminobutyl)piperidine (0.718 g, 4.6 mmol) dissolved in 3 mL dimethylformamide. This solution was then stirred at room temperature for 18 h, the volatiles were evaporated and the residue was diluted with water. Extraction with ethyl acetate followed by water and brine washes gave 1.40 g of an oil which was sufficiently pure for use in the next reaction. Mass spectrum, m+ =301.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05817676uspto-grants-1998_10