反応 #74911

反応方程式

Hydrogen chloride

5-chloro-1-indanone

chlorine

→

2,5-Dichloro-1-indanone

溶媒

acetic acid

反応条件

後処理

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

実験手順

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.

出典