Reaktion #7044

ord-4dd0bc4fe8c64d9e8f8801e446e2f232

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe mixture thus obtained
  2. 2
    workup.STIRRINGthe ultrasonic stirring
  3. 3
    Sonstigethe chloroform phase was separated
  4. 4
    Waschenwashed with a small amount of water
  5. 5
    Sonstigedried on Na2SO4
  6. 6
    Filtrationfiltered
  7. 7
    Einengenconcentrated to dryness
  8. 8
    SonstigeThe end product was isolated
  9. 9
    Sonstigepurified chromatographically on silica gel
  10. 10
    Wascheneluting with hexane

Vorschrift

ST 1385 1,1-di-indol-3-yl-butane, 290 mg (1 mmol), was thoroughly mixed and blended with potassium tertbutylate (280 mg) and tetrabutylammonium bromide (20 mg). The mixture thus obtained was held under ultrasonic stirring at ambient temperature. 640 mg (5 mmol) of benzylchloride at 0° C. were then added and the ultrasonic stirring was continued for 2 hours at room temperature. At the end of this period, the reaction mixture was treated with H2O/CHCl3; the chloroform phase was separated, washed with a small amount of water, dried on Na2SO4, filtered and concentrated to dryness. The end product was isolated and purified chromatographically on silica gel, eluting with hexane:ethyl ether 95:5.351 mg of product were obtained with a 78% yield.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07084166B2uspto-grants-2006_08