Process for preparing trifluoroethyl methacrylate
A technology of trifluoroethyl methacrylate and methacryloyl chloride, which is applied in the field of preparation of trifluoroethyl methacrylate, can solve the problems of high cost, low reaction capacity ratio, high risk of ether solvent, etc., and achieve The effect of stable product quality, mild reaction process conditions and cost reduction
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Embodiment 1
[0017] Add 10.0g (0.1mol) trifluoroethanol, 0.01g2,6-di-tert-butyl-p-cresol and 13.6g (0.13mol) methacrylic acid to the reactor equipped with heating, stirring, thermometer and reflux condenser Acyl chloride, stirred, the reaction temperature was controlled at 60-65 ° C, reacted for 8 hours, the obtained reaction solution was cooled to room temperature, washed with 5% sodium carbonate solution (weight percentage concentration) to neutrality, stirred for 1 hour, and decomposed in the reaction solution The side-reactants and excess methacryloyl chloride raw materials were washed with water, dried with anhydrous magnesium sulfate, filtered, and the obtained filtrate was distilled under reduced pressure to obtain 13.6g trifluoroethyl methacrylate with a yield of 81% and a purity of 99.2%. (HPLC), boiling point 100.8-101.2°C (literature value is 101°C),
[0018] IR (liquid film): 1740cm -1 , 1638cm -1 , 1350-1270cmu -1 , 1180-1135cm -1 , 980-945cm -1 .
Embodiment 2
[0020] Add 10.0g (0.1mol) trifluoroethanol, 0.01g2,6-di-tert-butyl-p-cresol and 14.6g (0.14mol) methacrylic acid to the reactor equipped with heating, stirring, thermometer and reflux condenser Acyl chloride, gradually heated and stirred, the reaction temperature was controlled at 50-70 ° C, reacted for 7 hours, the obtained reaction solution was cooled to room temperature, washed with 5% sodium carbonate solution (weight percentage concentration) to neutrality, stirred for 1 hour, and decomposed reaction The side reactants in the liquid and the excess methacryloyl chloride raw material were washed with water, dried with anhydrous magnesium sulfate, filtered, and the obtained filtrate was distilled under reduced pressure to obtain 13.7g trifluoroethyl methacrylate, with a yield of 81.5%, a purity of 99.3% (HPLC), boiling point 100.9-101.2°C.
Embodiment 3
[0022] Add 10.0g (0.1mol) trifluoroethanol, 0.01g2,6-di-tert-butyl-p-cresol, 14.6g (0.14mol) methacrylic acid to the reactor equipped with heating, stirring, thermometer and reflux condenser Acyl chloride, heating and stirring gradually, the reaction temperature is controlled at 40-60 ° C, reacted for 3 hours, and the reaction temperature was controlled at 60-80 ° C, reacted for 5 hours, the reaction solution obtained was cooled to room temperature, and was mixed with 5% sodium carbonate solution (weight percent concentration) to neutrality, stirred for 1 hour, decomposed side reactants in the reaction liquid and excessive methacryloyl chloride raw materials, washed with water, dried with anhydrous magnesium sulfate, filtered, and the obtained filtrate was distilled under reduced pressure to obtain 14.0g formazan Trifluoroethyl acrylate, yield 83.4%, purity 99.4% (HPLC), boiling point 100.9-101.2°C.
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