تفاعل #433279

ord-c14d5d24600e465890c68224b72d0d8d

المتفاعلات

الكواشف

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThen heat
  2. 2
    درجة الحرارةAfter cooling
  3. 3
    workup.ADDITIONpour the reaction mixture onto ice/hydrochloric acid
  4. 4
    أخرىseparate the organic phase
  5. 5
    استخلاصextract the aqueous phase with two portions of benzene
  6. 6
    غسيلWash the combined organic phases with water
  7. 7
    تجفيفdry with calcium chloride
  8. 8
    ترشيحfilter
  9. 9
    أخرىevaporate to dryness under vacuum
  10. 10
    أخرىRecrystallize the residue from methanol

الإجراء التجريبي

Heat 0.068 mol of iron(III) chloride to boiling in 20 ml of absolute benzene. Drop 0.0186 mol of 1-bromo-adamantane, dissolved in 30 ml of absolute benzene, to the solution. Then heat to boiling for 3 hrs. After cooling, pour the reaction mixture onto ice/hydrochloric acid, separate the organic phase, and extract the aqueous phase with two portions of benzene. Wash the combined organic phases with water, dry with calcium chloride, filter and evaporate to dryness under vacuum. Recrystallize the residue from methanol. (Yield: 80%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05061703uspto-grants-1991_10