New synthesis method of methyl fluoroacetate and ethyl fluoroacetate

A technology of ethyl fluoroacetate and methyl fluoroacetate, which is applied in the field of preparation of ethyl fluoroacetate, can solve the problems of low efficiency of ethyl fluoroacetate, low utilization rate of equipment, and low fluorinated reagents, and achieve simple post-processing procedures , High fluorination conversion rate, mild reaction conditions

Active Publication Date: 2021-06-08
宁夏森萱药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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 ...

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  • New synthesis method of methyl fluoroacetate and ethyl fluoroacetate

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Comparison scheme
Effect test

Embodiment 1

[0024] Such as figure 1 As shown, a new synthetic method of methyl fluoroacetate and ethyl fluoroacetate, the specific steps of the synthetic method are: feeding materials, putting methyl chloroacetate or ethyl chloroacetate into the reaction kettle, opening and stirring; adding catalyst, After stirring evenly, put in potassium fluoride, catalyst A, and catalyst B in turn, and close the feeding hole; heat, use heat transfer oil to heat up to 120°C, and start the reaction. After 1 hour, when the kettle temperature reaches 180°C and the kettle pressure reaches 0.8MPa , turn off the heat conduction oil heating, and start to keep warm; the temperature of the kettle and the pressure of the kettle rise slowly, and continue to keep warm for 3 hours. The material is press-filtered and rinsed, and the filtrate is rectified by a rectification tower to recover chloroacetate to obtain the product methyl fluoroacetate or ethyl fluoroacetate. The product quality can reach more than 99.5%. T...

Embodiment 2

[0031] Such as figure 1 As shown, a new synthetic method of methyl fluoroacetate and ethyl fluoroacetate, the specific steps of the synthetic method are: feeding materials, putting methyl chloroacetate or ethyl chloroacetate into the reaction kettle, opening and stirring; adding catalyst, After stirring evenly, put in potassium fluoride, catalyst A, and catalyst B in turn, and close the feeding hole; heat, use heat transfer oil to heat up to 120°C, and start the reaction. After 1 hour, when the kettle temperature reaches 180°C and the kettle pressure reaches 0.8MPa , turn off the heat conduction oil heating, and start to keep warm; the temperature of the kettle and the pressure of the kettle rise slowly, and continue to keep warm for 3 hours. The material is press-filtered and rinsed, and the filtrate is rectified by a rectification tower to recover chloroacetate to obtain the product methyl fluoroacetate or ethyl fluoroacetate. The product quality can reach more than 99.5%. T...

Embodiment 3

[0038] Such as figure 1 As shown, a new synthetic method of methyl fluoroacetate and ethyl fluoroacetate, the specific steps of the synthetic method are: feeding materials, putting methyl chloroacetate or ethyl chloroacetate into the reaction kettle, opening and stirring; adding catalyst, After stirring evenly, put in potassium fluoride, catalyst A, and catalyst B in turn, and close the feeding hole; heat, use heat transfer oil to heat up to 120°C, and start the reaction. After 1 hour, when the kettle temperature reaches 180°C and the kettle pressure reaches 0.8MPa , turn off the heat conduction oil heating, and start to keep warm; the temperature of the kettle and the pressure of the kettle rise slowly, and continue to keep warm for 3 hours. The material is press-filtered and rinsed, and the filtrate is rectified by a rectification tower to recover chloroacetate to obtain the product methyl fluoroacetate or ethyl fluoroacetate. The product quality can reach more than 99.5%. T...

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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...

Claims

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Application Information

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IPC IPC(8): C07C69/63C07C67/307C07C67/54
CPCC07C67/307C07C67/54C07C69/63
Inventor 林国平孙冬兵尹建炉
Owner 宁夏森萱药业有限公司
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