تفاعل #95205

ord-a51f038435e34d9bbc72f79b2f35dec5

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    ترشيحthe reaction mixture was filtered hot
  3. 3
    درجة الحرارةthe filtrate chilled
  4. 4
    أخرىYellow-green crystals formed
  5. 5
    أخرىwhich were recrystallized from 30 ml petroleum ether/15 ml acetone
  6. 6
    أخرىto give a white solid, mp 118°-128° C.

الإجراء التجريبي

A solution of alpha-hydroxyacetanilide (3.62 g, 0.024 mole), 4,4'-bis(N,N-dimethylamino)benzhydrol, methyl ether (6.81 g, 0.024 mole) 50 ml of tetrahydrofuran, 153 ml of n-hexane, and one drop of methanesulfonic acid was refluxed for 11 hours, during which time an additional 300 ml of solvent was added. The blue-green solution was decolorized with 4 drops of tetramethylguanidine and the reaction mixture was filtered hot and the filtrate chilled. Yellow-green crystals formed, which were recrystallized from 30 ml petroleum ether/15 ml acetone to give a white solid, mp 118°-128° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04343939uspto-grants-1982_08