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A kind of synthetic method of 2,6-dichloropyridine

A technology for dichloropyridine and a synthesis method, applied in the field of chemistry, can solve problems such as unsatisfactory selectivity of 2,6-dichloropyridine, and achieve the effects of prolonged reaction time, reduced speed and low energy consumption

Active Publication Date: 2017-04-12
盐城恒盛化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The addition of alkali undoubtedly brings extra work to the separation and purification of the product
In addition, the conversion rate of 2-chloropyridine and the selectivity of 2,6-dichloropyridine using this method are not ideal. Usually, the conversion rate of 2-chloropyridine is 32.9%, and the selectivity of 2,6-dichloropyridine is 87.2%. %

Method used

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  • A kind of synthetic method of 2,6-dichloropyridine
  • A kind of synthetic method of 2,6-dichloropyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 227 grams of 2-chloropyridine (2.0 moles) in a four-mouth jacketed glass reactor equipped with a reflux condenser, an air guide tube, a thermowell and a mechanical stirrer. Heating to 160°C, under the irradiation of 40W ultraviolet lamp, passing chlorine gas at a rate of 0.22mol / h for about 10 hours under normal pressure to react,

[0023] In the meantime, by Petite The oil bath circulation system realizes the temperature program of the reactor, so that the internal temperature of the reaction bottle gradually rises to 190°C. After the introduction of chlorine gas, the reaction solution was cooled to room temperature under a nitrogen atmosphere, and samples were taken for quantitative analysis by HPLC (the analysis results are shown in Table 1).

Embodiment 2

[0025] The reaction conditions were exactly the same as in Example 1, except that a 40W blue light was used as the light source (reaction results are shown in Table 1).

Embodiment 3

[0027] The reaction conditions are exactly the same as in Example 1, except that a 40W fluorescent lamp is used as the light source (reaction results are shown in Table 1).

[0028] Table 1. Chlorination reaction results using different light sources

[0029]

[0030]

[0031] a Trichloropyridine is a mixture of 2,3,6-trichloropyridine and 2,4,6-trichloropyridine; b Chlorine gas utilization refers to the ratio of the amount of chlorine gas consumed to generate 2,6-dichloropyridine to the total amount of chlorine gas introduced

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Abstract

The invention discloses a synthesis method of 2,6-dichloropyridine, which comprises the following step: reacting 2-chloropyridine or 2-chloropyridine hydrochloride and chlorine under photoinitiation actions at 160-190 DEG C to generate the 2,6-dichloropyridine. The invention provides a novel method for synthesizing 2,6-dichloropyridine, which is simple and efficient and has the advantages of no catalyst, no solvent, high conversion rate and high selectivity. After the reaction endpoint is reached, the obtained product does not need to be separated, purified or refined.

Description

technical field [0001] The invention relates to the technical field of chemistry, in particular to a synthesis method of 2,6-dichloropyridine. Background technique [0002] 2,6-Dichloropyridine is an important fine chemical intermediate, widely used in the fields of medicine and pesticide research. Pirozadil synthesized from 2,6-dichloropyridine can be used for lowering blood fat and anti-platelet aggregation. It can also be used to synthesize musk pyridine to replace natural musk. The 2,3,5,6-tetrachloropyridine produced by further chlorination of 2,6-dichloropyridine is an important raw material for the synthesis of chlorpyrifos, a highly efficient, broad-spectrum, and low-residue insecticide widely used in the world, and has a broad market. prospect. [0003] At present, the main synthetic routes of 2,6-dichloropyridine are: 1) Pyridine vapor phase high temperature or photocatalytic chlorination. The direct chlorination reaction conditions of pyridine are severe and e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 张小航程荣华
Owner 盐城恒盛化工有限公司
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