Method for preparing 2,3-dichloropyridine

A technology of dichloropyridine and aminopyridine is applied in the field of preparation of 2,3-dichloropyridine synthesis, can solve the problems of lack of large-scale production process, no large-scale production, etc., and achieves few steps, simple preparation process and high yield. high rate effect

Inactive Publication Date: 2015-09-23
ANHUI JIXI COUNTY HUIHUANG CHEM
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Problems solved by technology

[0002] 2,3-Dichloropyridine is an important fine chemical intermediate, which is widely used in the fields of medicine and pesticides, and is also the key to the new insecticide chlorantraniliprole For intermediates, due to the lack of mature large-scale production technology, there is no large-scale production in China. Exploring a reasonable and economical route is of great significance for industrialization guidance

Method used

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Embodiment Construction

[0014] A preparation method of 2,3-dichloropyridine, comprising the following steps:

[0015] (1) Add 55kg of 3-aminopyridine to the reaction kettle, add 560kg of 36% hydrochloric acid at one time, raise the temperature to 30-35°C, stir for about 20 minutes, dissolve the yellow transparent liquid, and cool down to Below 10°C (crystals will break out at low temperature); add 100kg of 30% hydrogen peroxide dropwise, drop it for 2 hours, keep warm for 2 hours below 10°C, and slowly rise to 25-30°C after the heat preservation, and keep at this temperature Insulated for 4 hours to generate 2-chloro-3-aminopyridine solution;

[0016] (2) Add 180 kg of 33% cuprous chloride hydrochloric acid solution to the 2-chloro-3-aminopyridine solution generated in the above (1), stir for about 10 minutes, and add 35% of ethylene oxide dropwise at 25-30°C Sodium nitrite aqueous solution 180kg, the initial reaction is violent, heat release is obvious, red gas is produced, it needs to be cooled w...

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Abstract

The invention provides a method for preparing 2,3-dichloropyridine. Reaction is conducted through adoption of raw auxiliary materials of 3-aminopyridine, hydrochloric acid, hydrogen peroxide, cuprous chloride, liquid caustic soda and the like, and the reaction principle is divided into three steps: firstly, 3-aminopyridine, hydrochloric acid and hydrogen peroxide react to generate 2-chlorine-3-aminopyridine, and 2-chlorine-3-aminopyridine is subjected to diazotization and Sandmeyer reaction so as to prepare the finished product. The method is simple in preparation process, less in step, relatively high in yield and high in purity.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a preparation method for synthesizing 2,3-dichloropyridine from 3-aminopyridine as a main 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. It is also the key intermediate of the new insecticide chlorantraniliprole. Due to the lack of mature large-scale production technology, there is no large-scale production process in China. Exploring a reasonable and economical route is of great significance to the guidance of industrialization. Contents of the invention [0003] The invention provides a preparation method of 2,3-dichloropyridine, which adopts 3-aminopyridine, hydrochloric acid, hydrogen peroxide, cuprous chloride, liquid caustic soda and other raw and auxiliary materials for reaction, and the reaction principle is divided into three steps: first, 3-amin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 戴汝平程捷朱良德
Owner ANHUI JIXI COUNTY HUIHUANG CHEM
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