반응 #64660

ord-2db01ce7b32a46519cdefc6ef82ad7c5

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Into a 500-mL, three-necked, round-bottomed flask, equipped with a magnetic stirrer
  2. 2
    온도heated
  3. 3
    온도under reflux with a heating mantle for 18 hours
  4. 4
    여과the mixture was filtered through a pad of Celite
  5. 5
    기타The clear filtrate was evaporated
  6. 6
    기타the residue was recrystallized from methanol

실험 절차

Into a 500-mL, three-necked, round-bottomed flask, equipped with a magnetic stirrer, a thermometer, and a condenser connected to a nitrogen bubbler, were placed carbazole (8.4 g, 50 mmole), allyl bromide (10 mL, 115 mmole), powdered anhydrous potassium carbonate (41 g, 300 mmole), and anhydrous acetonitrile (300 mL). The resultant mixture was stirred and heated under reflux with a heating mantle for 18 hours. Dichloromethane (300 mL) was then added, and the mixture was filtered through a pad of Celite. The clear filtrate was evaporated, and the residue was recrystallized from methanol to yield the desired product as amber-colored crystals. The product had melting point 56°-57° C., and sublimation (100° C./0.1 mm Hg) yielded white crystals (8.65 g, 83%), melting point 57°-58° C. The proton NMR spectrum in carbon tetrachloride was

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05414069uspto-grants-1995_05