Alpha-fluoropropionylacetate preparation method
A technology of fluoropropionoacetate and substituted propionoacetate, which is applied to the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., and can solve the problems of high equipment requirements, unfavorable industrial production, and safety problems. Low-level problems, to achieve the effect of low equipment requirements
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Embodiment 1
[0025]
[0026] Add 300 mL of anhydrous tetrahydrofuran to the dry reaction flask, cool to 0°C, add 13.1 g of 60% sodium hydride, and dropwise add 45.0 g of 1-fluoro-2-butanone, stir at 0°C for 30 minutes; then add dropwise at 0°C Dimethyl carbonate 60.0g, slowly warm up to room temperature (25°C) and continue to stir for 8h; GC detects that the reaction of raw materials is complete. Slowly add 100 mL of 1 mol / L hydrochloric acid to quench the reaction, evaporate most of the tetrahydrofuran under reduced pressure, extract the remaining reaction solution with 300 mL of ethyl acetate, separate the ethyl acetate layer, and wash with saturated sodium chloride solution. Dry over magnesium sulfate, concentrate the solvent to obtain a colorless oil, and then distill under reduced pressure to obtain 54.3 kg of a colorless transparent liquid with a yield of 73.3%.
[0027] 1 H NMR (300 MHz, CDCl 3 ) δ 5.04 (d, J = 48.5 Hz, 1H), 3.47 (s, 3H), 2.35 (q, J = 7.5 Hz, 2H), 0.68 (t, ...
Embodiment 2
[0030]
[0031] Add 500 mL of absolute ethanol to the dry reaction flask, cool to 0°C, add 100.0 g of sodium ethylate, and dropwise add 90.0 g of 1-fluoro-2-butanone, stir at 0°C for 30 minutes; then add dicarbonate dropwise at 0°C Ethyl ester 150.0g, slowly warm up to room temperature (25°C) and continue to stir for 12h; GC detects that the reaction of raw materials is complete. Slowly add 100 mL of 1 mol / L hydrochloric acid to quench the reaction, distill off most of the ethanol under reduced pressure, extract the remaining reaction solution with 500 mL of ethyl acetate, separate the ethyl acetate layer, and wash with saturated sodium chloride solution. Dry over magnesium sulfate, concentrate the solvent to obtain a colorless oil, and then distill under reduced pressure to obtain 82.9 g of a colorless transparent liquid with a yield of 65.7%.
[0032] 1 H NMR (300 MHz, CDCl 3 ) δ 5.20 (d, J = 49.3 Hz, 1H), 4.29 (q, J = 7.2Hz, 2H), 2.80-2.54 (m, 2H), 1.30 (t, J = 7...
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