Reaktion #335949

ord-03d5c0cd105e4024bc952133e486760d

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONTo a mixture of 30 g
  2. 2
    Sonstigeto react for 5 hours at 40° C.
  3. 3
    Temperaturthan at reflux temperature for 2 hours
  4. 4
    SonstigeThe solid was removed by filtration
  5. 5
    Einengenthe filtrate concentrated to dryness
  6. 6
    Sonstigeleaving a solid residue
  7. 7
    Waschenwashed twice with water
  8. 8
    ExtraktionThe organic extract
  9. 9
    Trocknenwas dried over sodium sulfate
  10. 10
    Sonstigeevaporated

Vorschrift

To a mixture of 30 g. potassium carbonate, 15 g. 1,2,4-triazole and 250 ml acetonitrile at 40° C. was added a solution of 45 g. 3,4-dihydro-2-bromo-1(2H)-naphthalenone in 150 ml acetonitrile. The mixture was allowed to react for 5 hours at 40° C. and than at reflux temperature for 2 hours. The solid was removed by filtration and the filtrate concentrated to dryness leaving a solid residue. This was dissolved in dichloromethane and washed twice with water. The organic extract was dried over sodium sulfate and evaporated to give 42 grams of product having a melting point of 96°-98° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05211736uspto-grants-1993_05