New hydrofluoro ether and its preparation method
A new technology of hydrofluoroether, which is applied in the field of new hydrofluoroether and its preparation, to achieve the effect of easy separation and purification, and increased yield
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example I
[0033] Example I: Effect of Solvent
example I-1
[0035] Dissolve 11.2g (0.2mol) of potassium hydroxide in 50g (0.5mol) of trifluoroethanol, add 100 grams of DMF solvent, seal in a 500mL autoclave, cool at low temperature, and introduce 130 grams (1.58mol) of trifluoroethylene in vacuum , heated to 78°C, and reacted for 6.5 hours. 89.2 grams of crude product were obtained by distillation, with a yield of 94.8%.
example I-2
[0037] Dissolve 11.2g (0.2mol) of potassium hydroxide in 50g (0.5mol) of trifluoroethanol, add 100 grams of DMSO solvent, seal in a 500mL autoclave, cool at low temperature, and introduce 130 grams (1.58mol) of trifluoroethylene in vacuum , heated to 78°C, and reacted for 6.5 hours. 87.3 grams of crude product were obtained by distillation, with a yield of 92.8%.
[0038] In the comparison of example I-1 and I-2, the yield is slightly higher than that of DMSO with DMF as the solvent. At the same time, during the distillation and purification process, DMSO has a partial decomposition phenomenon, which increases the loss of solvent and affects the purity of the product.
[0039] Because trifluoroethylene is a geometrically asymmetric structure, two isomers are formed when it is added to alcohol:
[0040] Chromatographic analysis shows that: when DMF and DMSO are used as solvents for the reaction, the product obtained by the addition of trifluoroethylene and trifluoroetha...
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