HRID46633

反应详情

EQUATION

反应方程式

HRID 46633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

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