تفاعل #74911

ord-bed636328b5147e69634a4632a778cba

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىto flow slowly into the solution at 10° C.
  2. 2
    أخرىto come gradually to room temperature
  3. 3
    workup.WAITAfter standing overnight
  4. 4
    workup.ADDITIONthe solution is poured onto ice
  5. 5
    استخلاصthe oil which separates out is extracted with acetic acid ethyl ester
  6. 6
    workup.DISTILLATIONthe solvent is distilled off under reduced pressure
  7. 7
    أخرىThe oil which remains crystallizes on standing
  8. 8
    أخرىThe product can be recrystallized from petroleum ether

الإجراء التجريبي

Hydrogen chloride gas is passed into a solution of 10.11 g (60 mmoles) of 5-chloro-1-indanone in 50 ml of glacial acetic acid at 10°-15° C. for 30 minutes. 4.25 g (60 mmoles) of condensed chlorine are then allowed to flow slowly into the solution at 10° C. and the mixture is allowed to come gradually to room temperature and is subsequently stirred for 3 hours. After standing overnight, the solution is poured onto ice, the oil which separates out is extracted with acetic acid ethyl ester and the solvent is distilled off under reduced pressure. The oil which remains crystallizes on standing. The product can be recrystallized from petroleum ether and then melts at 63°-66° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04174397uspto-grants-1979_11