Synthesizing method for ethyl difluoroacetate

A technology of ethyl difluoroacetate and a synthesis method, which is applied in the chemical industry, can solve the problems of low safety, complicated process, and high preparation cost, and achieve the effects of high safety, simple preparation method, and simple production steps

Inactive Publication Date: 2016-04-06
TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention proposes a synthetic method of ethyl difluoroacetate in order to solve the problems of comp

Method used

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  • Synthesizing method for ethyl difluoroacetate
  • Synthesizing method for ethyl difluoroacetate

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specific Embodiment approach 1

[0020] Specific implementation mode one: combine figure 1 Illustrate this embodiment mode, the synthetic method of a kind of ethyl difluoroacetate described in this embodiment mode is realized through the following steps:

[0021] Step 1. Preparation of the catalyst: Fill the tubular reactor with a certain number of Al 2 o 3 powder, ensure Al 2 o 3 The height of the powder is in the heating area of ​​the tube furnace, under the protection of nitrogen, heat to 250-300°C and keep it for 12h, and then continue to slowly feed CH a f b Cl c The gas reacts, the reaction temperature is 250-300°C, and the reaction time is 12h;

[0022] Step 2. Check the airtightness of the device and set the temperature control program; activate the catalyst at high temperature before adding raw materials, the activation temperature is 300 ° C, and the activation time is 3 hours. After the activation is completed, the temperature of the system drops to the set reaction temperature;

[0023] Ste...

specific Embodiment approach 2

[0027] Embodiment 2: The catalyst in step 2 of the synthesis method of ethyl difluoroacetate described in this embodiment is a Lewis acid catalyst AlFxCly. Other components and connections are the same as those in the first embodiment.

specific Embodiment approach 3

[0028] Specific embodiment three: the catalyst AlF of a kind of synthetic method of ethyl difluoroacetate described in this embodiment x Cl y The synthesis method is as follows:

[0029] Step A, fill 200 mesh Al in the tubular reactor 2 o 3 powder, and Al 2 o 3 The height of the powder in the heating zone of the tube furnace;

[0030] Step B, under the protection of nitrogen, heat to 250-300°C and keep for 12h;

[0031] Step C, continue to pass into CH a f b Cl c , where the values ​​of a, b, and c are 1 or 2 respectively, and the sum of a, b, and c is 4, and the reaction is carried out for 12h to obtain the catalyst AlF x Cl y The values ​​of x and y are uncertain integers, and the sum of x and y is 3. Other components and connections are the same as those in the second embodiment.

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Abstract

The invention relates to a synthesizing method, in particular to a synthesizing method for ethyl difluoroacetate, and aims at solving the problems that an existing synthesizing method for the ethyl difluoroacetate is complex in technological process, low in safety and high in preparation cost. The synthesizing method comprises the steps that 1, a catalyst is prepared, wherein a tubular reactor is filled with Al2O3 powder with the certain particle size meshes, it is guaranteed that the height of the Al2O3 powder is in a heating area of the tubular furnace, the temperature is increased to 250 DEG C-300 DEG C under nitrogen protection and kept for 12 h, CHaFbClc gas is continuously and slowly introduced for a reaction, the reaction temperature is set at 250 DEG C-300 DEG C, and the reaction time is set for 12 h; 2, 1,1,2,2-tetrafluoroethyl ethylether is taken as raw materials for a reaction under the conditions of the certain temperature and the catalyst, and an intermediate does not need to be separated and is directly collected through condenser to be converted into ethyl ester. The method belongs to the field of chemical engineering.

Description

technical field [0001] The invention relates to a synthesis method, in particular to a synthesis method of ethyl difluoroacetate, which belongs to the field of chemical industry. Background technique [0002] The molecular formula of ethyl difluoroacetate is: CHF 2 COOC 2 h 5 , is a transparent or light yellow liquid, aromatic and slightly irritating, slightly soluble in water, miscible with organic solvents, and easily decomposed when exposed to water. It is a new type of pharmaceutical and pesticide intermediate with a promising market prospect. [0003] According to bibliographical reports, the main technique of preparing ethyl difluoroacetate at present has: (1) synthetic difluoroacetic acid with tetrafluoroethylene raw material, the main shortcoming of this technique is that tetrafluoroethylene belongs to inflammable and explosive on the one hand, and is difficult for transportation, It needs to be used on site; on the other hand, the cost is relatively high. (2) Ta...

Claims

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Application Information

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IPC IPC(8): C07C69/63C07C67/08
CPCC07C51/58C07C67/08C07C53/48C07C69/63
Inventor 相继欣郭海强闫锐肖山
Owner TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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