تفاعل #74911
ord-bed636328b5147e69634a4632a778cba
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىto flow slowly into the solution at 10° C.
- 2أخرىto come gradually to room temperature
- 3workup.WAITAfter standing overnight
- 4workup.ADDITIONthe solution is poured onto ice
- 5استخلاصthe oil which separates out is extracted with acetic acid ethyl ester
- 6workup.DISTILLATIONthe solvent is distilled off under reduced pressure
- 7أخرىThe oil which remains crystallizes on standing
- 8أخرىThe 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.