New synthesis method of methyl fluoroacetate and ethyl fluoroacetate

Abstract

The invention discloses a novel synthesis method of methyl fluoroacetate and ethyl fluoroacetate. The method comprises the following specific steps: adding methyl chloroacetate or ethyl chloroacetate into a reaction kettle, and starting stirring; after uniformly stirring, sequentially adding potassium fluoride, a catalyst A and a catalyst B, and closing a charging hole; heating to 120 DEG C by using heat-conducting oil, starting reaction, stopping heating by the heat-conducting oil and starting heat preservation when the kettle temperature reaches 180 DEG C and the kettle pressure reaches 0.8 MPa after 1 hour; after keeping heat preservation for 3 hours and the kettle temperature reaches 220 DEG C and the kettle pressure reaches 1.5 MPa, continuously preserving heat for 5 hours; and cooling to 80 DEG C, discharging, carrying out filter pressing, rinsing, rectifying filtrate through a rectifying tower, and recovering chloroacetate to obtain the product methyl fluoroacetate or ethyl fluoroacetate, the product quality can reach 99.5% or above, and the molar yield (metered by potassium fluoride) reaches 96% or above. The method has the advantages of mild reaction conditions, simple operation, easy control, high fluoro conversion rate, high product yield, simple post-treatment process, realization of solvent-free reaction, and low energy consumption.

Description

technical field [0001] The invention relates to the field of preparation methods of ethyl fluoroacetate, in particular to a new synthesis method of methyl fluoroacetate and ethyl fluoroacetate. Background technique [0002] Methyl fluoroacetate is an important fluorine-containing compound, which has a wide range of uses and development prospects in the industrial fields of dyestuffs, medicines, and pesticides. In the pharmaceutical industry, ethyl fluoroacetate is an important pharmaceutical intermediate. It is the starting material for the preparation of fluoropyrimidine antineoplastic drugs and fluoroquinolate antibacterial drugs. . Ethyl fluoroacetate and methyl fluoroacetate are important pharmaceutical intermediates for the synthesis of 5-fluorouracil and 5-fluorocytosine. At present, domestic production of ethyl fluoroacetate mostly uses chloroacetate and fluorinating reagents, such as potassium fluoride, sodium fluoride, etc. for fluorination, and the reaction formu...

AI Technical Summary

Problems solved by technology

Due to the low activity of fluorinated reagents, the excess of fluorinated reagents in production is often 10-20%, and the reaction process requires organic solvents, resulting in low utilization of equipment and low yield between 45-80%. Most of the separation adopts rectification, and the purity of the product can reach more than 95%.

[0003]The existing production technology of ethyl fluoroacetate has the disadvantages of low efficiency, high cost, high energy consumption, serious pollution, etc., and the development of green and efficient production method is particularly important

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