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Method for synthesizing 2,6-diamino pyridine

A diaminopyridine and synthesis method technology, applied in the field of 2,6-diaminopyridine synthesis, can solve the problems of low synthesis process yield and many by-products, and achieve good product selectivity, easy operation, and simple process Effect

Inactive Publication Date: 2014-09-03
姜树林
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the yield of the synthesis process of 2,6-diaminopyridine is relatively low, and there are many by-products. Therefore, it is of great research significance to improve the yield and purity of the product

Method used

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  • Method for synthesizing 2,6-diamino pyridine
  • Method for synthesizing 2,6-diamino pyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] In the autoclave, add 1mol of 2,6-dichloropyridine, the activated loading capacity is 10% nano-ruthenium carbon catalyst and 800 ml of quinoline, close the autoclave, feed 20mol of liquid ammonia, close After the reactor, the temperature was raised to 350 ° C, and the reaction was stirred for 12 hours. After the reaction, the excess liquid ammonia was drained, 300 ml of water was added, stirred and cooled to 0-5 ° C, 89 g of solids were obtained by filtration, and 99.1% of The 2,6-diaminopyridine product was 81.8 grams, with a melting point of 121.1-122.3°C and a yield of 75%.

Embodiment 2

[0017] Add 1mol of 2,6-bromochloropyridine in the autoclave, the nanometer ruthenium carbon catalyst and the quinoline of 800 milliliters through the activated loading capacity of 10%, close the high pressure reactor, pass into 20mol of liquid ammonia, close After the reactor, the temperature was raised to 350°C and the reaction was stirred for 12 hours. After the reaction, excess liquid ammonia was drained, 300 milliliters of water was added, stirred and cooled to 0-5°C, filtered to obtain 95 grams of solid, and purified with toluene to obtain 99.3% of 2 , 83.5 grams of 6-diaminopyridine product, melting point 121.3-122.5°C, yield 76.6%.

Embodiment 3

[0019] Add 1mol of 2,6-bromochloropyridine in the autoclave, the nanometer ruthenium carbon catalyst and the quinoline of 800 milliliters through the activated loading capacity of 10%, close the autoclave reactor, pass into the liquid ammonia of 20mol, close After the reactor, the temperature was raised to 350 ° C, and the reaction was stirred for 12 hours. After the reaction, the excess liquid ammonia was drained, 300 ml of water was added, stirred and cooled to 0-5 ° C, 102 g of solids were obtained by filtration, and 99.3% of 92.8 g of 2,6-diaminopyridine product, melting point 122.3-122.7°C, yield 85.1%.

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Abstract

The invention discloses a method for synthesizing 2,6-diamino pyridine, which is characterized by comprising the following steps of: in a high-pressure reactor, adding 2,6-dihalogenated pyridine, solvent and catalyst; closing the high-pressure reactor; filling liquid ammonia; reacting at temperature of 200-1000 DEG C to obtain a crude product; and refining by methyl benzene to obtain the target product. The method for synthesizing 2,6-diamino pyridine has the advantages that the method is simple in process, easy in operation and excellent in product selectivity; and the product purity is greater than 99%, and total yield is 75-85%.

Description

technical field [0001] The invention relates to a synthesis method of 2,6-diaminopyridine. Background technique [0002] 2,6-Diaminopyridine is a traditional organic chemical product, which is mainly used in high-end fine chemicals such as medicine and pesticides. In addition, this product is also used in hair dyeing products, because the hair dyeing products synthesized by this product as an intermediate have better light resistance. At present, the yield of the synthesis process of 2,6-diaminopyridine is relatively low, and there are many by-products. Therefore, it is of great research significance to improve the yield and purity of the product. Contents of the invention [0003] The purpose of this invention is to provide a kind of synthetic method of 2,6-diaminopyridine. [0004] In order to solve the above-mentioned technical problems, the technical scheme adopted in the present invention is: a synthetic method of aminopyridine, which is characterized in that: in th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/73
Inventor 王德峰张耀兵王炳才张燕程石飞
Owner 姜树林
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