preparation | synthesis method of dimethyl 2, 2-dimethylmalonate: a synthesis method of dimethyl 2, 2-dimethylmalonate: weigh 104.2g of 2, 2-dimethyl-1, 3-propanediol and 0.2g of Phosphotungstic acid as catalyst, add to 340g of 50% hydrogen peroxide solution in batch with constant stirring, oxidize it to 2, the crude solution of 2, 2-dimethylmalonic acid had a molar ratio of 2, 2-dimethyl-1, 3-propanediol to hydrogen peroxide of 1:5. Concentrated and acidified, and after cooling, crystals of 2, 2-dimethylmalonic acid were obtained. The crystals were filtered with suction and recrystallized with deionized water to obtain a pure product of 2, 2-dimethylmalonic acid with a yield of 86%. Then, sodium bisulfate monohydrate was used as a catalyst, and the amount added was 10% of the mass of 2, 2-dimethylmalonic acid. 2, 2-dimethylmalonic acid was esterified with methanol, and cyclohexane was used as a water-carrying agent. Methanol and 2, The molar ratio of 2-dimethylmalonic acid is 6:1, the reaction temperature is 70-75 ° C., and the reaction time is 2-4 hours. After the reaction, the cyclohexane and methanol were distilled off, and the liquid was applied. The crude product, dimethyl 2, 2-dimethylmalonate, was washed with water, separated, dried with anhydrous magnesium sulfate, and distilled under reduced pressure with an oil pump, the 106-110 ° C. Fractions were collected to obtain dimethyl 2, 2-dimethylmalonate in a yield of 96%. The purity was 99.96%. |