Reaktion #1090485

ord-6ead61ed7f334ccbbe9f4b782457297e

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with water
  2. 2
    Trocknena saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate
  3. 3
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure
  4. 4
    SonstigeThe residue thus obtained
  5. 5
    Sonstigewas chromatographed over a silica gel column

Vorschrift

To a suspension of 0.055 g of 6-(4-ethyl-1-piperazinyl)pyridine-3-carboxamide, 0.011 g of tetrabutylammonium hydrogen sulfate, 0.11 g of sodium hydroxide and 0.05 g of potassium carbonate in 3 ml of toluene was added dropwise at 70° C. a solution of 12-bromododecanol in 2 ml of toluene and the mixture was stirred at 70° C. for 13 hours. The reaction solution was diluted with chloroform, washed with water and a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The residue thus obtained was chromatographed over a silica gel column to afford 0.025 g of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06046201uspto-grants-2000_04