91526-18-0

80841-78-7

91526-18-0

Example 4 Preparation of 4-hydroxymethyl-5-methyl-1,3-dioxolan-2-one: 4-chloromethyl-5-methyl-1,3-dioxolan-2-one (50 g) was dissolved in acetonitrile (500 ml), and formic acid (45 g) was slowly added at 20-25 °C. The reaction mixture was then cooled to 10-15 °C and triethylamine (95 g) was added. The reaction system was heated to 60-65°C and the reaction was kept at this temperature with stirring for 5-6 hours. After completion of the reaction, the mixture was cooled to 15-20 °C, filtered and the filter cake was washed with acetonitrile. The filtrates were combined and the acetonitrile was removed by distillation under reduced pressure to concentrate the solution. The concentrated reaction was cooled to 25-30 °C, ethyl acetate and water were added and stirred at 25-30 °C for 15-20 minutes. The aqueous layer was separated, the aqueous layer was extracted with ethyl acetate, the organic layers were combined and washed with brine. The organic layer was separated and evaporated to dryness at 35-40°C under reduced pressure. Methanol was added to the residual oil and heated to reflux temperature. Isopropanol solution of HCl was added dropwise and the reaction was refluxed for 60-75 minutes. At the end of the reaction, it was cooled to 30-35 °C and distilled under reduced pressure to remove all solvent to give 4-(hydroxymethyl)-5-methyl-[1,3]dioxolen-2-one as an oily product (yield: 34.6 g; yield: 79%).