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Preparation of 2-chloro-3-pyridinamine

A technology of aminopyridine and production method, which is applied in the field of 2-chloro-3-aminopyridine, can solve the problems of aggravated environmental pollution, difficult separation, unsatisfactory yield, etc., and achieve the effects of reducing raw material costs, avoiding pollution, and low cost

Active Publication Date: 2011-01-12
ABA CHEM CORP
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Problems solved by technology

[0003] 1) take 2,3,6-trichloropyridine as raw material, under catalyst platinum, ruthenium, carry out hydrogenation catalytic reaction and make, and this method has detailed record in the Japanese patent that Patent Publication No. is H01-1193246, but this method The cost of the catalyst used is high and not suitable for industrial production
[0004] 2) Synthesize 2,3-dichloropyridine with 2-chloropyridine as a raw material. The product obtained by this method contains 2,3-dichloropyridine and 2,5-dichloropyridine at the same time, and the separation is difficult and the yield is not ideal
[0008] This method will inevitably produce a large amount of by-product 2,6-dichloro-3-aminopyridine (about 2-chloro-3-amino 10~15% of pyridine), so, not only the yield of 2-chloro-3-aminopyridine is low, and produce a large amount of waste 2,6-dichloro-3-aminopyridine, increase the processing cost of solid waste and increase the weight of environmental pollution

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  • Preparation of 2-chloro-3-pyridinamine

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Embodiment Construction

[0019] The following are specific examples of the present invention to further describe the technical solution of the present invention in detail, but the present invention is not limited to the examples.

[0020] According to the production method of the 2-chloro-3-aminopyridine of the present embodiment, comprises the steps:

[0021] (1), the aqueous solution of 3-aminopyridine is cooled to 0 ℃, feeds 80g (2.2mol) dry hydrogen chloride, then at 0~5 ℃, adds 17.6g 46% (0.24mol) hydrogen peroxide within 2 hours, makes reaction The system was reacted at 15-20°C for 3 hours to obtain a mixture containing 2-chloro-3-aminopyridine and 2,6-dichloro-3-aminopyridine.

[0022] 12 ml of 30% sodium sulfite solution, 200 ml of water, 50 ml of toluene and 82 g of 50% sodium hydroxide solution were added to the mixture and the layers were separated. The aqueous layer is washed with ten parts of 50ml toluene, and the obtained toluene washing liquid is removed to obtain the by-product 2,6-di...

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Abstract

The invention relates to a preparation of 2-chloro-3-pyridinamine, which comprises the step(1): performing chlorination reaction onto 3-pyridinamine as raw material in the presence of perhydrol and hydrochloric acid to obtain the 2-chloro-3-pyridinamine and by-product of 2, 6-dichlor-3-pyridinamine, in particular, the preparation further comprises the step (2): carrying out catalytic hydrogenation reaction onto the by-product of 2, 6-dichlor-3-pyridinamine to generate the 3-pyridinamine used as raw material. The preparation of the invention is low in cost and pollution, and is applicable forcommercial process.

Description

technical field [0001] The invention relates to a method for producing 2-chloro-3-aminopyridine by using 3-aminopyridine as raw material. Background technique [0002] 2.3-Dichloropyridine is an important fine chemical intermediate, which is widely used in the fields of medicine and pesticides, such as the preparation of crop protection agents. In the prior art, the preparation of 2,3-dichloropyridine mainly contains the following three kinds: [0003] 1) take 2,3,6-trichloropyridine as raw material, under catalyst platinum, ruthenium, carry out hydrogenation catalytic reaction and make, and this method has detailed record in the Japanese patent that Patent Publication No. is H01-1193246, but this method The catalyst used has high cost and is not suitable for industrial production. [0004] 2) 2,3-dichloropyridine is synthesized by using 2-chloropyridine as a raw material. The product obtained by this method contains both 2,3-dichloropyridine and 2,5-dichloropyridine, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/73B01J23/755B01J23/44B01J27/13
Inventor 印湘湘林靖阙利民蔡彤
Owner ABA CHEM CORP
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