반응 #335949

ord-03d5c0cd105e4024bc952133e486760d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONTo a mixture of 30 g
  2. 2
    기타to react for 5 hours at 40° C.
  3. 3
    온도than at reflux temperature for 2 hours
  4. 4
    기타The solid was removed by filtration
  5. 5
    농축the filtrate concentrated to dryness
  6. 6
    기타leaving a solid residue
  7. 7
    세척washed twice with water
  8. 8
    추출The organic extract
  9. 9
    건조was dried over sodium sulfate
  10. 10
    기타evaporated

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05211736uspto-grants-1993_05