Preparation method of trifluoroacetamidine

A kind of technology of trifluoroacetamidine and trifluoroacetamide, applied in the field of preparation of trifluoroacetamidine

Inactive Publication Date: 2012-11-21
JIANGSU TETRA NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] The purpose of this invention is to provide a kind of preparation method of important chemical intermediate trifluoroacetamidine, this method has solved the problem that adopts the stronger gas substance of toxicity as raw material, makes trifluoroacetonitrile by selecting more suitable method, and Further obtain trifluoroacetamidine, the product selectivity and productive rate are higher, more conducive to industrialized production

Method used

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  • Preparation method of trifluoroacetamidine
  • Preparation method of trifluoroacetamidine

Examples

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Embodiment 1

[0014] (1) Preheat polyphosphoric acid at 50°C to increase its fluidity;

[0015] (2) Add 100Kg trifluoroacetamide, 170Kg phosphorus pentoxide and 200L polyphosphoric acid to a 1000L gas reactor respectively, stir at a constant speed, and slowly raise the temperature to 150°C, and the gas produced immediately is trifluoroacetonitrile;

[0016] (3) Pour trifluoroacetonitrile into a 500L liquid ammonia kettle after cooling, keep the reaction temperature at -40 to -35°C, and stop the reaction after stirring for 3 hours;

[0017] (4) Recycling and processing excess liquid ammonia, distilling the remaining raffinate under reduced pressure, collecting 35-37°C / 11mmHg fraction to obtain a colorless liquid, which is the product trifluoroacetamidine, the product purity is higher than 95%, and the yield is higher than 85%.

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Abstract

The invention relates to a preparation method of trifluoroacetamidine. The trifluoroacetamidine is an important chemical intermediate with wide purposes. A preparation method comprises the following steps that trifluoroacetamide is used as raw materials, polyphosphoric acid is selected as solvents under the effect of phosphorus pentoxide as dehydrating agents, trifluoroacetonitrile can be fast prepared through dehydration reaction, the generated trifluoroacetonitrile gas is introduced into a liquid ammonia kettle after being cooled, and the trifluoroacetamidine can be prepared. When the method is used for preparing the trifluoroacetamidine, various problems caused when the trifluoroacetonitrile gas with high toxicity is directly adopted as raw materials are avoided, the production risk is reduced, meanwhile, the operation difficulty is also reduced, the product yield is also improved, in addition, the preparation method has the advantages that the production process is simple, the product yield and the product purity are higher, and the like. The preparation method is suitable for industrial production.

Description

technical field [0001] The invention relates to an important chemical intermediate trifluoroacetamidine, in particular to a preparation method of trifluoroacetamidine. Background technique [0002] Trifluoroacetamidine, the molecular formula is C 2 f 3 N 2 h 3 , the structural formula is . [0003] Trifluoroacetamidine is an important synthetic intermediate, which can be used in the synthesis of nitrogen-containing heterocyclic compounds or various amidine compounds, and many amidine compounds can be used as medicines. In addition, amidine is also the main component of formamidine UV absorbers, the NH or NH of amidine 2 After one or more Hs are substituted by substituents, various ultraviolet absorbers with excellent performance will be formed. Therefore, trifluoroacetamidine is widely used in medicine, chemical industry, pesticide and other fields. The R&D and production of trifluoroacetamidine were carried out earlier in foreign countries, but the industrial produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C257/14
Inventor 韩建伟常杨军曹祥来曹祥明
Owner JIANGSU TETRA NEW MATERIAL TECH
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