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Method for synthesizing 3,3,3-trifluoro methyl propionate

A technology of methyl trifluoropropionate and a synthesis method, applied in the field of chemistry, can solve the problems of few reaction steps, low reaction yield, complicated post-processing and the like, and achieves less loss of intermediate products, wide sources and simple post-processing Effect

Active Publication Date: 2013-06-12
XIAN MODERN CHEM RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the technical problems of many reaction steps, low yield and complex post-treatment in the background technology, the purpose of the present invention is to provide a 3,3,3- The synthetic method of methyl trifluoropropionate

Method used

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  • Method for synthesizing 3,3,3-trifluoro methyl propionate

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preparation example Construction

[0021] According to the technical scheme of the present invention, the synthetic method of 3,3,3-trifluoromethyl propionate of the present invention specifically comprises the steps:

[0022] (1) Put methanol, Pd / C catalyst, and pro-oxidant in the reaction kettle, feed 3,3,3-trifluoropropene and oxygen, heat up to 70°C~120°C, react for 8h~12h, cool, and put The reaction solution is filtered, and the filtrate is used in the next step, wherein, the mass ratio of 3,3,3-trifluoropropene: Pd / C catalyst: methanol: pro-oxidant is 1: 1.4~2.5: 0.02~0.2: 0.04~0.4; Pd / The palladium content of C catalyst is 5% of catalyst gross mass, and prooxidant is cupric chloride or ferric chloride;

[0023] (2) Add the filtrate, protonic acid and pro-oxidant obtained in step (1) into a three-necked flask, raise the temperature to 60°C~80°C, add 30% hydrogen peroxide dropwise, and then react at 60°C~80°C for 4h~ 8h; the reaction solution was filtered and distilled, and the fraction at 70°C~73°C was ...

Embodiment 1

[0029] (1) Put 20g of methanol, 0.26g of Pd / C catalyst, and 1.33g of copper chloride in an autoclave, and feed 13g of raw material 3,3,3-trifluoropropene at -50°C, and then pass After adding 1MPa oxygen, heat up to 120°C with stirring, react for 8 hours, cool to room temperature, slowly release the gas in the system, open the kettle, filter the reaction solution, separate and remove the catalyst, and the filtrate is used in the next step.

[0030] (2) Put 25g of the reaction solution obtained in step (1) into a three-necked flask, add 1.9g of hydrochloric acid and 0.5g of vanadium pentoxide, raise the temperature to 60°C, and slowly add 9g of hydrogen peroxide with a mass fraction of 30% under stirring In the reaction flask, react for 6h. The reaction solution was filtered and distilled at atmospheric pressure, and the fraction at 70~73°C was collected to obtain 11.9 g of methyl 3,3,3-trifluoropropionate with a purity of 97%. The total yield of the two steps is 59.8%.

Embodiment 2

[0032] (1) Put 20g of methanol, 0.5g of Pd / C catalyst, and 1.33g of ferric chloride in a high-pressure reactor, inject 13g of raw material 3,3,3-trifluoropropene at -50°C, and inject 1MPa After oxygen, the temperature was raised to 100°C with stirring, and the reaction was carried out for 24 hours. After the reaction, cool to room temperature, slowly release the gas in the system, open the kettle to discharge, filter the reaction solution, separate and remove the catalyst, and the filtrate is used in the next step.

[0033] (2) Put 25g of the filtrate obtained in step (1) into a three-necked flask, add 2.2g of hydrochloric acid and 1.5g of vanadium pentoxide, heat up to 80°C, and slowly add 18g of hydrogen peroxide with a mass fraction of 30% under stirring In the reaction flask, react for 4h. The reaction solution was filtered and distilled at atmospheric pressure, and the fraction at 70~73°C was collected to obtain 11.9 g of methyl 3,3,3-trifluoropropionate with a purity of...

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Abstract

The invention discloses a method for synthesizing 3,3,3-trifluoro methyl propionate. The method comprises the following steps of: putting 3,3,3-trifluoropropene serving as a raw material, methyl alcohol, a Pd / C catalyst and a pro-oxidant in a reaction kettle, after introducing 3,3,3-trifluoropropene and oxygen gas, heating up to the temperature of 70-120 DEG C, reacting for 8-12 hours, cooling and filtering reacted liquid; and adding obtained filtrate, protonic acid and the pro-oxidant into a three-neck flask, heating up to the temperature of 60-80 DEG C, dropwise adding hydrogen peroxide, and reacting for 4-8 hours, thereby obtaining 3,3,3-trifluoro methyl propionate. The method has the advantages that the few synthesizing steps (only two steps) are carried out, the yield is high, and the after-treatment is simple.

Description

technical field [0001] The invention belongs to a synthesis method in the field of chemistry, and in particular relates to a synthesis method of 3,3,3-trifluoromethyl propionate. Background technique [0002] Methyl 3,3,3-trifluoropropionate can be used as an intermediate in the synthesis of medicines and pesticides, and can also be used as a raw material or intermediate in the synthesis of high-performance fluorine-containing materials. For example, "Convenient synthesis of 3,3,3-trifluoropropanoic acid by hydrolytic oxidation of 3,3,3-trifluoropropanaldimethyl acetate" Journal of fluorine chemistry, 129 (1) 35-39, 2008 discloses a 3,3,3-trifluoro The preparation method of methyl propionate, the method uses 3,3,3-trifluoropropenyl ether as raw material to prepare the method of 3,3,3-trifluoropropionate methyl ester through three-step reaction, the synthetic route of this method is as follows: [0003] [0004] First, 3,3,3-trifluoropropenyl ether and methanol are cataly...

Claims

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Application Information

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IPC IPC(8): C07C69/63C07C67/39
Inventor 亢建平吕剑杜咏梅郝志军毛伟张建伟王伟杨志强李亚妮王志轩秦越韩升
Owner XIAN MODERN CHEM RES INST
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