Reaktion #524232

ord-1943a5d681f645c9b0b00ea880096c00

Reaktionsbedingungen

Temperatur
85°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool to ambient temperature
  2. 2
    SonstigeThe solvent is removed
  3. 3
    Sonstigeleaving a yellow semi-solid which
  4. 4
    Extraktionextracted into ether
  5. 5
    ExtraktionThe ether extract
  6. 6
    Waschenis washed with water
  7. 7
    Sonstigedried
  8. 8
    Filtrationfiltered
  9. 9
    Sonstigethe solvent removed

Vorschrift

A solution of 8.0 g of 2-(2-cyclopropylamino)acetyl-1-(o-fluorobenzyl)pyrrole, free base of a, in 100 ml of isopropyl alcohol is added to a suspension of 2.2 g sodium borohydride in 100 ml of isopropanol. The reaction mixture is refluxed at 85° C. for 4 hours, allowed to cool to ambient temperature and 50 ml of methanol introduced. The solvent is removed leaving a yellow semi-solid which is treated with water and then extracted into ether. The ether extract is washed with water, dried and filtered and the solvent removed leaving a pure yellow oil of 2-(cyclopropylamino)-1-[1-(o-fluorobenzyl)-2-pyrryl]ethanol. Infrared and nuclear magnetic resonance spectra confirm this structure.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04029672uspto-grants-1977_06