Reaktion #64722

ord-0208c64273a84e8e8c4fda96508a2f39

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    TemperaturThe mixture was heated
  3. 3
    Temperaturunder reflux for 3.5 hours
  4. 4
    Filtrationinsoluble substances were filtered off
  5. 5
    EinengenThe filtrate was concentrated
  6. 6
    Extraktionthe residue was subjected to extraction with the addition of water and ethyl acetate
  7. 7
    SonstigeThe organic layer was separated
  8. 8
    Extraktionthe aqueous layer was then extracted with ethyl acetate
  9. 9
    Trocknendried over anhydrous magnesium sulfate
  10. 10
    SonstigeThe solvent was evaporated off under reduced pressure
  11. 11
    Sonstigethe residue was purified by silica gel chromatography

Vorschrift

In 50 ml of tetrahydrofuran were dissolved 1.5 g of 1-(2-chlorophenyl)piperazine and 5 ml of triethylamine, and 3.4 g of 2-[bis(4-hydroxyphenyl)methyl]benzylbromide was added thereto. The mixture was heated under reflux for 3.5 hours, and then insoluble substances were filtered off. The filtrate was concentrated, and the residue was subjected to extraction with the addition of water and ethyl acetate. The organic layer was separated, and the aqueous layer was then extracted with ethyl acetate. The organic layers were combined and then dried over anhydrous magnesium sulfate. The solvent was evaporated off under reduced pressure, and the residue was purified by silica gel chromatography to afford 0.54 g of the desired compound (Compound 89).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05413997uspto-grants-1995_05