Preparation method for 4,5-difluoro-1,3-dioxolan-2-one
A technology of difluoroethylene carbonate and dichloroethylene carbonate is applied in the synthesis field of difluoroethylene carbonate, can solve the problems of low conversion rate, low yield, complex reaction components, etc. Corrosion and decomposition, easy solid-liquid separation, high reaction conversion rate
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Embodiment 1
[0025] Take by weighing 157g (1mol) dichloroethylene carbonate, 64g fluorinating agent pyridine trifluoride ( ) was dissolved in a reaction vessel of 400ml ether, and 120g of acid-binding agent pyridine was added dropwise at -10°C for 1 hour, and after the addition was completed, it was kept at 10-20°C for 2 hours, filtered, and the filtrate was distilled off under normal pressure to remove ether to obtain diethyl ether. The crude fluoroethylene carbonate was distilled under reduced pressure to obtain 99 g of difluoroethylene carbonate with a purity of 99.92%, and the yield was 80.58%.
Embodiment 2
[0027] Take by weighing 157g (1mol) dichloroethylene carbonate, 65g fluorinating agent triethylamine trihydrogen fluoride (Et 3 N·3HF) was dissolved in 400ml of tetrahydrofuran in a reaction vessel, and 145g of acid-binding agent triethylamine was added dropwise at -5°C for 1 hour, and after the addition was completed, it was kept at 10-20°C for 2 hours, filtered, and the filtrate was distilled under normal pressure The solvent was removed to obtain a crude product of difluoroethylene carbonate, which was then distilled under reduced pressure to obtain 105.5 g of difluoroethylene carbonate with a purity of 99.94%, with a yield of 85%.
Embodiment 3
[0029] Take by weighing 1570g (10mol) dichloroethylene carbonate, 660g fluorinating agent triethylamine trihydrogen fluoride (Et 3 N·3.5HF) was dissolved in a reaction vessel of 4500ml methyl tert-butyl ether, and 1500g of acid-binding agent triethylamine was added dropwise at -5°C for 2.5 hours. After filtration, the filtrate was distilled under normal pressure to remove the solvent to obtain crude difluoroethylene carbonate, and then distilled under reduced pressure to obtain 1100 g of difluoroethylene carbonate with a purity of 99.96%, with a yield of 88.7%.
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