반응 #442804

ord-bbb9b5d1220b4263bb77e16a751e72f6

반응 조건

온도
20°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the solution heated for 2 hours
  2. 2
    온도under reflux
  3. 3
    여과filtration
  4. 4
    workup.ADDITIONthe red filtrate added dropwise to 1000 pbv of 0.5% strength ammonia solution
  5. 5
    여과the precipitate was filtered off by suction
  6. 6
    기타crystallized from 135 pbv of ethanol

실험 절차

5.68 pbw of 2-amino-9-(4-methylphenyl)acridine (compound 12d) were dissolved with 20.3 pbw of methanesulfonyl chloride and 22.4 pbw of diazabicyclo[2.2.2]octane in 120 pbv of acetonitrile and the solution heated for 2 hours under reflux. After cooling to 20° C., filtration was carried out and the red filtrate added dropwise to 1000 pbv of 0.5% strength ammonia solution. After standing overnight, the precipitate was filtered off by suction and crystallized from 135 pbv of ethanol. Yield: 1.76 pbw (20% of theory), light yellow needles. Mp.: 217°-219° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05834157uspto-grants-1998_11