Synthetic method for vinyl ethylene carbonate
A technology of vinyl ethylene carbonate and synthesis method, which is applied in the field of chemical synthesis, can solve the problems of multiple by-products, difficult purification, extreme toxicity, etc., and achieve the effects of easy post-processing, good selectivity, and less side reactions
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Embodiment 1
[0038] First, 130 g of bis(chloroform) carbonate was dissolved in 400 g of dichloromethane. Add 88g of butylene glycol and 320g of pyridine to the dry reaction flask, control the reaction temperature at 5°C, and slowly add the above-prepared dichloromethane solution of bis(trichloromethane)carbonate dropwise to the reaction flask under stirring . After the dropwise addition, continue to stir and react at this temperature for 0.5 hour. After the reaction is completed, add an appropriate amount of water, stir, leave to stand for stratification, separate the lower organic layer, dry the organic layer with anhydrous magnesium sulfate, and remove the solvent. Finally, the product vinyl ethylene carbonate was extracted by fractional distillation under reduced pressure to obtain 100 g of vinyl ethylene carbonate crude product with a yield of 87.7% and a gas chromatography analysis purity of 98.5%.
Embodiment 2
[0040] First, 125 g of bis(chloroform) carbonate was dissolved in 500 g of dichloroethane. Add 88g of butenediol, 10g of pyridine, and 420g of triethylamine to the dry reaction flask, control the reaction temperature at 10°C, and slowly add the above-prepared bis(chloroform) carbonate to the reaction flask dropwise under stirring solution of dichloroethane. After the dropwise addition, continue to stir the reaction at this temperature for 0.5 hours, and then stir the reaction at room temperature for 1 hour. After the reaction is completed, add an appropriate amount of water, stir, stand and separate the layers, and separate the lower organic layer. Anhydrous magnesium sulfate was dried, and after removing the solvent, the product vinyl ethylene carbonate was extracted by vacuum fractional distillation to obtain 95 g of vinyl ethylene carbonate crude product with a yield of 83.3% and a gas chromatography analysis purity of 98.8%.
Embodiment 3
[0042] First, 120 g of bis(chloroform) carbonate was dissolved in 600 g of benzene. Add 88g of butenediol and 450g of pyridine to the dry reaction flask, control the reaction temperature at 15°C, and slowly add the above-prepared benzene solution of bis(trichloromethane)carbonate dropwise to the reaction flask under stirring. After the dropwise addition, continue to stir and react at this temperature for 1.5 hours. After the reaction, add an appropriate amount of water, stir, leave to stand for layering, and separate the upper organic layer. The organic layer is dried with anhydrous magnesium sulfate. After removing the solvent, Finally, the product vinyl ethylene carbonate was extracted by vacuum fractional distillation to obtain 88 grams of vinyl ethylene carbonate crude product with a yield of 77.2% and a gas chromatography analysis purity of 98.2%.
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