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Preparation method of fluoroacetate

A technology of fluoroacetate and chloroacetate, which is applied in the preparation of fluoroacetate and the preparation of fine chemical products, and can solve the problems of low efficiency of fluoroacetate, low activity of fluorinated reagents, and low utilization rate of equipment, etc. problems, achieve high conversion efficiency, simple post-processing procedures, and save materials

Inactive Publication Date: 2013-03-20
王学军
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] 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%.
[0006] The existing production technology of fluoroacetate has shortcomings such as low efficiency, high cost, high energy consumption, and serious pollution. It is particularly important to develop green and efficient production methods

Method used

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  • Preparation method of fluoroacetate

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Embodiment 1

[0028] The preparation of embodiment 1 potassium fluoride solid dispersion:

[0029] (1), add 1000g of water to the container, under stirring, add 600g of potassium fluoride to the water, stir until completely dissolved;

[0030] (2), under stirring, add micropowder silica gel 60g in the aqueous solution of potassium fluoride, continue to stir for 45 minutes;

[0031] (3) Remove moisture by rotary evaporation, and dry to obtain 661.5 g of a solid dispersion of potassium fluoride.

[0032] After testing, the potassium fluoride content in the solid dispersion is 89.7%, the moisture content is 0.12%, and the specific surface area is 165m 2 / g.

Embodiment 2

[0033] The preparation of embodiment 2 ethyl fluoroacetates:

[0034] Add 122 g of ethyl chloroacetate to the container, add 65 g of potassium fluoride solid dispersion under stirring, react at 20° C. for 3 hours, and separate to obtain 103 g of ethyl fluoroacetate with a yield of 99.1% and a purity of 99.7%.

Embodiment 3

[0035] The preparation of embodiment 3 ethyl fluoroacetates:

[0036] Add 122 g of ethyl chloroacetate to the container, add 65 g of potassium fluoride solid dispersion under stirring, react at 25° C. for 5 hours, and separate to obtain 100 g of ethyl fluoroacetate with a yield of 98.4% and a purity of 99.8%.

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Abstract

The invention relates to a preparation method of fluoroacetate. The invention adopts a solid disperse technology to prepare a potassium fluoride solid dispersion, so that potassium fluoride exists in the form of extremely tiny crystal grains or molecules on the surface of a micropowder silica gel, has a very large specific area, and thus is highly active. The fluoroacetate is prepared from chlorochloracetate and the potassium fluoride solid dispersion under very mild condition, and the preparation method of fluoroacetate is high in fluorine conversion rate, simple in post treatment, and good in finished product quality, and has unexpected effects and very good application prospect.

Description

technical field [0001] The invention relates to a preparation method of fine chemical products, in particular to a preparation method of fluoroacetate, which belongs to the technical field of chemical industry. Background technique [0002] Ethyl fluoroacetate (CAS No.: 459-72-3) and Methylfluoroacetate (CAS No.: 453-18-9) are important pharmaceutical intermediates for the synthesis of 5-fluorouracil, 5- Flucytosine. At present, most domestically produced fluoroacetates use chloroacetate and fluorinating reagents, such as potassium fluoride and sodium fluoride, for fluorination. The reaction formula is as follows: [0003] [0004] where R=-CH 3 、-C 2 h 5 . [0005] 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 is rectification, and the purity of the pro...

Claims

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Application Information

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IPC IPC(8): C07C67/307C07C69/63
Inventor 李瑞菊王学军陈子雷丁蕊艳方丽萍
Owner 王学军
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