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ChemicalBook CAS DataBase List Fluoroethylene carbonate
114435-02-8

Fluoroethylene carbonate synthesis

7synthesis methods
The preparation of Fluoroethylene carbonate is as follows:Add 114g of liquid ethylene carbonate at 50, 1.14g of palladium acetate (II) and 114g of dry acetonitrile (water 100ppm) to a 500ml Monel reactor containing the monophenyl iodine difluoride prepared in step (1) , Stir at 50°C for 0.5h, raise the temperature to 70°C and react for 5h (the molar ratio of ethylene carbonate to hydrogen fluoride in step (1) is 1.1:2.5, the molar ratio of ethylene carbonate to acetonitrile is 1.1:2.8, palladium acetate (II) The dosage is 1.0% of the mass of ethylene carbonate). The tail gas during the reaction was absorbed by potassium hydroxide solution with a mass fraction of 10%. After the reaction, vacuum distillation was carried out under the condition of 3mmHg. The 65-71°C fraction was collected to obtain 103.3g of fluoroethylene carbonate with a GC content of 99.3%. The yield of FEC was 75%.
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Yield:114435-02-8 98.2%

Reaction Conditions:

with N-fluorobis(benzenesulfon)imide at 120; for 0.5 h;Sealed tube;Reagent/catalyst;

Steps:

2 example 2

Into a sealed reactor, 100 g of ethylene carbonate and 370 g of N-fluorobistrifluoromethanesulfonamide were added and stirred, and the temperature was raised to 120°C. HPLC analysis until the reaction time of ethylene carbonate was undetectable , the reaction time was 0.9 h, and the reaction was stopped. The fluoroethylene carbonate product was separated by distillation and had a purity of >99.9% and a yield of 97.8%.the chroma was 8 Hazen. Replace the above fluorinated reagent with 390 g of N-fluorobisbenzenesulfonamide. Under the same conditions, the complete reaction time was 1/2 h, the purity was >99.9%, the yield was 98.2%, and the chroma was 8 Hazen.

References:

CN108033943,2018,A Location in patent:Paragraph 0020; 0024; 0025

Fluoroethylene carbonate Related Search:

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