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Preparation method for fluoromalonic acid diester

A technology of fluoromalonate diester and fluoroacetate ester is applied in the field of preparation of fluoromalonate diester, and can solve the problems of strong corrosion of equipment, high requirement of reaction equipment, environmental pollution and the like

Inactive Publication Date: 2018-04-20
LANZHOU CHEMSPECWEIER CHEM CO LTD
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  • Claims
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AI Technical Summary

Problems solved by technology

The main disadvantages of this method are that the raw materials are highly toxic, highly corrosive to equipment, and have high requirements for reaction equipment. Dichloromalonate and difluoromalonate diester will be produced during the reaction process, which will affect product quality and yield.
In addition, in the post-treatment process, triethylamine is difficult to recover and a large amount of nitrogen-containing wastewater is generated, which is troublesome to deal with and causes great pollution to the environment.
[0005] In addition, Chinese patent (CN 1025318) provides a method for preparing diethyl fluoromalonate, which uses ethyl fluoroacetate and diethyl oxalate as initial raw materials, and synthesizes them through two steps of condensation and oxidation Diethyl fluoromalonate, the total yield is 32.5%. This method still has the problems of low yield and many "three wastes"

Method used

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  • Preparation method for fluoromalonic acid diester
  • Preparation method for fluoromalonic acid diester
  • Preparation method for fluoromalonic acid diester

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preparation example Construction

[0027] The invention provides a kind of preparation method of fluoromalonate diester (formula III compound), and described preparation method comprises:

[0028] Condensation reaction of fluoroacetate (compound of formula I) and dialkyl carbonate (compound of formula II) in the presence of alkali to prepare fluoromalonate diester, said formula I, formula II, The structural formula of the compound of formula III is as follows:

[0029]

[0030] In the preparation method provided by the present invention, R1, R2, and R3 can be independently selected from alkyl groups, more specifically, for example, C1~C6 alkyl groups, C1~C3 alkyl groups, etc. In a specific embodiment of the invention, The R1, R2 and R3 may be independently selected from methyl or ethyl. In another specific embodiment of the present invention, the groups of R1, R2 and R3 are the same.

[0031] In the preparation method provided by the present invention, the base can generally provide alkaline conditions in ...

Embodiment 1

[0041] Preparation of dimethyl fluoromalonate:

[0042] In a 250ml round bottom flask, add 80.0g dimethyl carbonate and 5.4g sodium methoxide, heat to reflux, add 9.0g methyl fluoroacetate dropwise, and react for 2h. Use 30% hydrochloric acid to adjust PH=6~7 to quench the reaction, separate the liquid, and distill the organic phase under reduced pressure to obtain 8.3 g of dimethyl fluoromalonate (content 96.5%), with a yield of 54.6%.

Embodiment 2

[0044] Preparation of dimethyl fluoromalonate:

[0045] In a 250ml round bottom flask, add 40g tetrahydrofuran, 40.0g dimethyl carbonate and 10.8g sodium methoxide, heat to reflux, drop 9.0g methyl fluoroacetate, and react for 4h. The reaction was quenched with 30% hydrochloric acid, separated, and the organic phase was distilled under reduced pressure to obtain 8.3 g of dimethyl fluoromalonate (content: 94.2%), with a yield of 53.3%.

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Abstract

The invention especially relates to a preparation method for fluoromalonic acid diester, belonging to the field of organic synthesis. The preparation method comprises a step of subjecting fluoroacetate and dialkyl carbonate to a condensation reaction in the presence of alkali so as to prepare fluoromalonic acid diester. The preparation method provided by the invention is mild in reaction process;the preparation method has low toxicity and corrosivity due to elimination of conventional chlorination and fluorination steps; and the preparation method does not produce difluoromalonic acid diesterimpurities, has low requirements on factory equipment and is simple and safe to operate.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of fluoromalonate diester. Background technique [0002] Fluoromalonate diester is an important class of fluorine-containing organic intermediates, which can undergo a series of reactions such as alkylation, alkoxylation, and hydroxyalkylation. It is widely used in organic synthesis, medicine, pesticides, and spices. , dyes, etc., therefore, fluoromalonate diester derivatives have an extremely broad field and very broad development prospects, and it is of great significance to develop a high-efficiency, low-cost fluoromalonate diester synthesis process . [0003] At present, the methods for preparing fluoromalonate diester mainly include the following: carbonyl elimination method, esterification method, cracking method and fluorination method. [0004] At present, most domestic manufacturers adopt the hydrogen fluoride salt fluorination method. That is, us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/313C07C69/63
CPCC07C67/313C07C69/63
Inventor 顾竞何立袁云龙杜友兴
Owner LANZHOU CHEMSPECWEIER CHEM CO LTD
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