Synthetic method for 2-picolinic acid

A technology of picolinic acid and synthesis method, which is applied in the direction of organic chemistry, can solve the problems of a large amount of waste liquid, pollute the environment, and equipment corrosion, and achieve the effects of less by-products, lower reaction temperature, and easy separation

Inactive Publication Date: 2017-09-15
ANHUI XINGYU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chemical oxidation method mostly uses potassium permanganate, selenium dioxide or potassium dichromate as the oxidant, which is a relatively mature synthesis method, but the method is costly, and a large amount of waste liquid will be generated during the production process, which will pollute the environment and corrode the equipment. serious

Method used

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  • Synthetic method for 2-picolinic acid

Examples

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Comparison scheme
Effect test

Embodiment 1

[0026] 1, a kind of synthetic method of 2-picolinic acid, comprises the following steps:

[0027] (1) Dicyclopentadienyl cobalt, manganese acetate and cobalt acetate are added to the reactor with a mass ratio of 10:2:1 as a catalyst and acetonitrile, and dry acetylene is introduced at room temperature until the pressure of the reactor rises to 1.1MPa, Stir and heat up to 145°C, react for 9.5 hours, concentrate the reaction solution, and purify by rectification to obtain 2-picoline;

[0028] (2) Heating the above-mentioned 2-picoline on a heating bed to 350-370°C to turn into steam, then mix it with ammonia, water vapor and air, and catalyze oxidation through the catalyst layer to obtain 2-pyridinecarbonitrile, The catalyst layer includes a catalyst, a promoter and a catalyst carrier, the catalyst is germanium oxide, antimony trioxide and vanadium oxide, the promoter is copper and zirconium, and the catalyst carrier is alumina;

[0029] (3) Add the above-mentioned 2-pyridineca...

Embodiment 2

[0031] 1, a kind of synthetic method of 2-picolinic acid, comprises the following steps:

[0032] (1) Add dicyclopentadienyl cobalt, manganese acetate and cobalt acetate into the reactor with a mass ratio of 10:2:1 as a catalyst and acetonitrile, feed dry acetylene at room temperature until the pressure of the reactor rises to 1MPa, stir Raise the temperature to 150°C, react for 9 hours, concentrate the reaction solution, and purify by rectification to obtain 2-picoline;

[0033] (2) Heating the above-mentioned 2-picoline on a heating bed to 350-370°C to turn into steam, then mix it with ammonia, water vapor and air, and catalyze oxidation through the catalyst layer to obtain 2-pyridinecarbonitrile, The catalyst layer includes a catalyst, a promoter and a catalyst carrier, the catalyst is germanium oxide, antimony trioxide and vanadium oxide, the promoter is copper and zirconium, and the catalyst carrier is alumina;

[0034] (3) Add the above-mentioned 2-pyridinecarbonitrile ...

Embodiment 3

[0036] Substantially the same as Example 1, the difference is that the reactor pressure is 0.8MPa in step (1), the temperature is 140°C, and the reaction is 8h; the concentration of sodium hydroxide solution in step (3) is 40%, and the temperature is raised to 70°C The reaction was stirred for 5h, cooled to room temperature and then stirred for 5h.

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Abstract

The invention provides a synthetic method for 2-picolinic acid, belonging to the field of organic chemical synthesis. The synthetic method comprises the following steps: adding acetonitrile and a catalyst composed of cobaltocene, manganese acetate and cobalt acetate into a reaction vessel, introducing acetylene at room temperature and carrying out stirring and heating for a reaction so as to prepare 2-methylpyridine; heating 2-methylpyridine with a heating bed so as to turn 2-methylpyridine into steam, then mixing the 2-methylpyridine steam with ammonia gas, water vapor and air and carrying out catalytic oxidation via a catalyst layer so as to prepare 2-pyridinecarbonitrile; and adding 2-pyridinecarbonitrile into a sodium hydroxide solution, successively carrying out heating, stirring reaction, cooling to room temperature and pumping filtration, washing a filter cake and carrying out drying and crystallization so as to obtain 2-picolinic acid. The synthetic method provided by the invention has the advantages of high yield, simple production process, easiness in product separation and low production of waste gas, waste water and industrial residues.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a method for synthesizing 2-pyridinecarboxylic acid. Background technique [0002] The molecular formula of picolinic acid is: C5H5NO2. In structure, it also contains Lewis acid and Lewis basic functional groups, and is a typical heterocyclic amphoteric compound. Picolinic acid series are widely used in medicine, chemical industry, food and life, and have irreplaceable functions and values. Therefore, scholars and experts at home and abroad have carried out a lot of research on the synthesis of picolinic acid. Picolinic acid includes α, β, and γ three isomers: picolinic acid, niacin and isonicotinic acid. [0003] Among them, α-picolinic acid is called 2-picolinic acid. 2-picolinic acid is an important intermediate in organic synthesis. Intermediates such as drugs are widely used in nerve suppression and local anesthesia, and the market demand is large. 2-Picolinic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/16C07D213/12C07D213/84C07D213/80C07D213/803
CPCC07D213/16C07D213/12C07D213/80C07D213/803C07D213/84
Inventor 张升张宽宇金文艺李静
Owner ANHUI XINGYU CHEM
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