HRID2422392
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
The hydrochloride 4-(8-phenyl-1,4-dioxaspiro[4,5]dec-8-yl)pyrrolidine hydrochloride (5.8 g, 17.9 mmol) was dissolved in 7.5N hydrochloric acid (16 ml) and stirred for 24 h at room temperature. On completion of hydrolysis the reaction mixture was extracted with diethyl ether (2×50 ml), the aqueous phase was made alkaline using 5N sodium hydroxide solution with ice cooling, extracted with dichloromethane (3×50 ml) and concentrated to small volume. The ketone 4-pyrrolidin-4-yl-4-phenylcyclohexanone was able to be isolated as a yellow solid with a melting point of 75-79° C. and a yield of 96% (4.1 g).
WORKUP
后处理
- customOn completion of hydrolysis the reaction mixture
- extractionwas extracted with diethyl ether (2×50 ml)
- extractionextracted with dichloromethane (3×50 ml)
- concentrationconcentrated to small volume
- customto be isolated as a yellow solid with a melting point of 75-79° C.