反应详情

4-(8-Phenyl-1,4-dioxaspiro[4.5]dec-8-yl)pyrrolidine hydrochloride (5.8 g, 17.9 mmol) was dissolved in 7.5 N hydrochloric acid (16 ml) and the mixture was stirred at room temperature for 24 h. When the hydrolysis had ended, the reaction mixture was extracted with diethyl ether (2×50 ml), and the aqueous phase was rendered alkaline with 5 N sodium hydroxide solution, while cooling with ice, and extracted with methylene chloride (3×50 ml) and the extract was concentrated. It was possible to isolate the ketone Ket-8 as a yellow solid with a melting point of 75-79° C. and a yield of 96% (4.1 g).

1. extractionthe reaction mixture was extracted with diethyl ether (2×50 ml)
2. temperaturewhile cooling with ice
3. extractionextracted with methylene chloride (3×50 ml)
4. concentrationthe extract was concentrated