反应详情

[8-(3-Fluoro-phenyl)-1,4-dioxa-spiro[4.5]dec-8-yl]-dimethyl-amine hydrochloride (7.2 g, 22.75 mmol) was dissolved in water (9.6 ml), concentrated hydrochloric acid (14 ml, 455 mmol) was added and the mixture was stirred at room temperature for 4 d. 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, during which the product precipitated out. It was possible to isolate the ketone Ket-13 as a yellow solid with a melting point of 83-88° C. and a yield of 50% (6.05 g).

1. extractionthe reaction mixture was extracted with diethyl ether (2×50 ml)
2. temperaturewhile cooling with ice, during which the product
3. customprecipitated out