HRID1179029
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- washThe reaction mixture was washed three times with 50 ml diethyl ether each time
- extractionextracted three times with 100 ml methylene chloride each time
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationthe filtrate was concentrated