58012-34-3

62141-26-8

58012-34-3

To acetone (720 mL) was added 10 g (43.8 mmol, 1 eq.) of ethyl (1,4-dioxaspiro[4.5]dec-8-yl)acetate followed by 1 N hydrochloric acid (180 mL). The reaction mixture was heated to reflux for 2 hours. After completion of the reaction, it was cooled to room temperature, diluted with ethyl acetate (100 mL) and washed with deionized water (100 mL). The aqueous layer was back-extracted twice with ethyl acetate (100 mL), all the organic layers were combined, dried with anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure to give 7.57 g (94% yield) of ethyl 4-oxocyclohexaneacetate as a clear oil. The product was characterized by 1H-NMR (CDCl3): δ 4.16 (q, 2H), 2.40 (m, 4H), 2.32 (m, 2H), 2.28 (m, 1H), 2.10 (m, 2H), 1.49 (m, 2H), 1.28 (t, 3H); TLC Rf = 0.32 (unfolding reagent ratio of ethyl acetate/hexanes 3:7).