To a round-bottomed flask containing a solution of THF:MeOH (50 mL, 1:5, v/v) with KOH (46.46 mmol) was slowly added 2,2,5,5-tetramethyl-1,3-dioxane-4,6-dione (11.61 mmol) at 0 °C. The reaction mixture was stirred at room temperature for 24 hours. After completion of the reaction, the mixture was poured into a solution of 1 M HCl (50 mL) and extracted with ether. The organic phases were combined, washed with saturated brine, dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to give monomethyl 2,2-dimethylmalonate in 88% yield.
