HRID1179029

反应详情

EQUATION

反应方程式

HRID 1179029 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

165 ml hydrochloric acid (32 wt. %) were diluted with 100 ml water, 60.0 g dimethyl-(8-phenyl-1,4-dioxa-spiro[4.5]dec-8-yl)-amine were added to this approx. six molar hydrochloric acid and the mixture was stirred for 24 hours. The reaction mixture was washed three times with 50 ml diethyl ether each time, rendered alkaline (pH>10) with 100 ml sodium hydroxide solution (32 wt. %) and extracted three times with 100 ml methylene chloride each time. The extracts were combined, dried over sodium sulfate and filtered and the filtrate was concentrated. 36.1 g 4-dimethylamino-4-phenyl-cyclohexanone were obtained.

WORKUP

后处理

  1. washThe reaction mixture was washed three times with 50 ml diethyl ether each time
  2. extractionextracted three times with 100 ml methylene chloride each time
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated