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Method and device for preparing methyl fluoroacetate

A technology of methyl fluoroacetate and methyl chloroacetate, which is applied in the preparation of methyl fluoroacetate and the field of equipment for preparing methyl fluoroacetate, can solve the problems of low purity and yield of methyl fluoroacetate, and improve the reaction conversion The efficiency, the process is simple and reasonable, and the effect of improving the reaction yield

Active Publication Date: 2015-01-21
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of this invention is to provide a kind of preparation method of methyl fluoroacetate, solve the problem that the purity and yield of methyl fluoroacetate obtained by the existing preparation method are lower

Method used

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  • Method and device for preparing methyl fluoroacetate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preparation method of the methyl fluoroacetate of present embodiment, comprises the following steps:

[0026] 1) Add 223kg of potassium fluoride, 494kg of dimethylformamide (DMF), 333kg of acetamide and 10kg of catalyst dodecyltrimethylammonium bromide into the reaction kettle. Under normal pressure, start the stirring tank to stir, and heat up;

[0027] 2) Add 434 kg of methyl chloroacetate into the raw material storage tank. When the temperature of the reactor rises to 100°C, continue to add methyl chloroacetate into the reactor at a rate of 10 kg / min for reaction, and at the same time condense the two Condensed water is fed into the condenser respectively, and the mixed gas generated by the reaction enters the two-stage condenser for two-stage condensation;

[0028] 3) According to the difference in boiling point temperature, methyl chloroacetate and methyl fluoroacetate in the mixed gas are condensed in the first and second condensers of the two-stage condenser...

Embodiment 2

[0034] The preparation method of the methyl fluoroacetate of present embodiment, comprises the following steps:

[0035] 1) Add 500kg of potassium fluoride, 700kg of dimethylformamide (DMF), 500kg of acetamide and 20kg of catalyst tetrabutylammonium chloride into the reaction kettle. Under normal pressure, start the stirring tank to stir and raise the temperature;

[0036] 2) Add 1000kg of methyl chloroacetate to the raw material storage tank. When the temperature of the reactor rises to 160°C, continue to add methyl chloroacetate into the reactor at a rate of 5kg / min for reaction, and simultaneously condense the two Condensed water is fed into the condenser respectively, and the mixed gas generated by the reaction enters the two-stage condenser for two-stage condensation;

[0037]3) According to the difference in boiling point temperature, methyl chloroacetate and methyl fluoroacetate in the mixed gas are condensed in the first and second condensers of the two-stage condenser...

Embodiment 3

[0041] The preparation method of the methyl fluoroacetate of present embodiment, comprises the following steps:

[0042] 1) Add 1000kg of potassium fluoride, 800kg of dimethylformamide (DMF), 500kg of acetamide and 30kg of catalyst tetrabutylammonium bromide into the reaction kettle. Under normal pressure, turn on the stirring tank to stir and raise the temperature;

[0043] 2) Add 1000kg of methyl chloroacetate to the raw material storage tank. When the temperature of the reactor rises to 130°C, continue to add methyl chloroacetate into the reactor at a rate of 10kg / min for reaction. At the same time, the two-stage condensation Condensed water is fed into the condenser respectively, and the mixed gas generated by the reaction enters the two-stage condenser for two-stage condensation;

[0044] 3) According to the difference in boiling point temperature, methyl chloroacetate and methyl fluoroacetate in the mixed gas are condensed in the first and second condensers of the two-st...

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Abstract

The invention discloses a method and device for preparing methyl fluoroacetate. The preparation method comprises the following steps of (1) adding potassium fluoride, a solvent and a catalyst in a reaction kettle, stirring and heating; (2) adding methyl chloroacetate into the reaction kettle continuously to carry out reaction when the temperature rises to a reaction temperature, performing two-stage condensation on a mixed gas generated by the reaction, wherein methyl chloroacetate in the mixed gas is condensed to form a liquid in a first stage and returned to the reaction kettle to participate the reaction continuously and methyl fluoroacetate is condensed to form a liquid in a second stage to form the product, according to difference of boiling temperatures. According to the preparation method provided by the invention, the obtained methyl fluoroacetate product has high purity; and the technology process is simple and reasonable, has relatively high reaction conversion rate and yield, can be operated and controlled easily, and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of methyl fluoroacetate, specifically relates to a method for preparing methyl fluoroacetate, and also relates to a device for preparing methyl fluoroacetate. Background technique [0002] Fluoroacetate is an important class of pharmaceutical intermediates. It is the basic raw material for the preparation of anti-tumor drug fluoropyrimidine, antibacterial drugs such as 5-fluorouracil, fluoxic acid, cyprofluxacil, and furoxazine. Pesticides, dyes, spices intermediates. At present, the production method of fluoroacetate in industry is mainly: under the condition of aprotic solvent, chloroacetate is reacted with potassium fluoride, and fluoroacetate is obtained after separation. Since the fluorination reaction requires a higher temperature and a longer reaction time, in the existing industrial production, the one-time extensive feeding method leads to the inability of the fluorination reaction to fully proceed...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/63C07C67/307
CPCC07C67/307C07C69/63
Inventor 侯红军杨华春司腾飞薛旭金杨明霞师玉萍邹英武贺志荣姚超
Owner DO FLUORIDE CHEM CO LTD
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