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Preparation method of substituted pyridine

A technology of pyridine and cyanopyridine, applied in the field of preparation of substituted pyridine, can solve the problems of high price of 2-vinylpyridine, hinder industrial application, unsatisfactory recycling effect, etc., and achieve the effect of saving energy

Active Publication Date: 2020-06-23
杭州瑞思新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the price of 2-vinylpyridine used in this method is high, and the recycling effect is not ideal, which hinders industrial application

Method used

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  • Preparation method of substituted pyridine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) In a jet loop reactor based on the Venturi effect, the operating principle is based on the Venturi effect, the loop operates as downward flow, and the jet mixer 1 end of the reactor is immersed in the liquid phase of the loop reactor, First carry out nitrogen replacement, then add 10 mol of acrylic acid and 10 mol of 4-cyanopyridine through the material feed port 5 in sequence, and turn on the external circulation pump 3 at 70°C for high-speed jet mixing.

[0030] 2) Control the temperature at 70°C, slowly add 10 mol of hydrogen chloride raw material into the injection loop reactor through the gas raw material feed port 6, and spray and mix through the jet mixer 1 to achieve a sufficient reaction between the materials, and the feeding time is 2 hour, after the addition finished, after the injection loop reactor continued to react for 2 hours, the first step reaction ended;

[0031] 3) After the first step of the reaction is completed, the temperature of the system is...

Embodiment 2

[0038] 1) In a jet loop reactor based on the Venturi effect, the operating principle is based on the Venturi effect, the loop operates as downward flow, and the jet mixer 1 end of the reactor is immersed in the liquid phase of the loop reactor, First carry out nitrogen replacement, then add 15 mol of acrylic acid and 10 mol of 4-cyanopyridine through the material feed port 5 in sequence, and turn on the external circulation pump 3 at 110°C for high-speed jet mixing.

[0039] 2) Control the temperature at 110°C, slowly add 15 mol of hydrogen chloride raw material into the injection loop reactor through the gas raw material feed port 6, and spray and mix through the jet mixer 1 to achieve a sufficient reaction between the materials, and the feeding time is 1 hour, after the feed ended, after the injection loop reactor continued to react for 1 hour, the first step reaction ended;

[0040] 3) After the first step of the reaction is completed, the temperature of the system is lower...

Embodiment 3

[0047] 1) In a jet loop reactor based on the Venturi effect, the operating principle is based on the Venturi effect, the loop operates as downward flow, and the jet mixer 1 end of the reactor is immersed in the liquid phase of the loop reactor, First carry out nitrogen replacement, then add 12 mol of acrylic acid and 10 mol of 4-cyanopyridine sequentially through the material feed port 5, and turn on the external circulation pump 3 at 90°C for high-speed jet mixing.

[0048] 2) Control the temperature at 90°C, slowly add 13 mol of hydrogen chloride raw material into the injection loop reactor through the gas raw material feed port 6, and spray and mix through the jet mixer 1 to achieve a sufficient reaction between the materials, and the feeding time is 1.5 hour, after the feed ended, after the injection loop reactor continued to react for 1.5 hours, the first step reaction ended;

[0049] 3) After the first step of reaction is completed, the temperature of the system is lower...

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Abstract

The invention discloses a preparation method of substituted pyridine. The method is implemented in a jet loop reactor based on a Venturi effect. First nitrogen displacement is performed, then, acrylicacid and 4-cyanopyridine raw materials are sequentially added through a material feeding opening; an outer circulating pump is started at 70 to 110 DEG C for high-speed spraying and mixing; a hydrogen chloride raw material is slowly added into the jet loop reactor through a gas raw material feeding hole; spraying and mixing are performed through a spraying type mixer, and full reaction among materials is realized; and the like. According to the method, a novel jet loop reactor based on the Venturi effect is adopted; a traditional stirred tank reactor is replaced; according to the reactor, themass transfer among various reaction species in the reactor is greatly promoted, so that the reaction can be dynamically controlled, and when reaction raw materials are sprayed and pushed forwards under the action of the pump, strong suction force can be generated to automatically suck gas-phase reaction materials in the reaction kettle, so that an excellent mass transfer effect is obtained in violent turbulent flow.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a preparation method of substituted pyridines. Background technique [0002] Pyridine functional groups widely exist in drug molecules and functional materials, and are an important class of heterocyclic structures. Most of the traditional methods for synthesizing substituted pyridine derivatives require the participation of transition metal catalysts or metal organic reagents, and the scope of application is limited by their respective characteristics. Therefore, how to realize the synthesis or functionalization of pyridine compounds through simple and effective methods is an important issue. [0003] 4-Dimethylaminopyridine (DMAP for short) is a super nucleophilic acylation catalyst. 4-Dimethylaminopyridine is a new type of high-efficiency catalyst widely used in chemical synthesis in recent years. The electron-donating dimethylamino in its structure resonates wi...

Claims

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Application Information

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IPC IPC(8): C07D213/74
CPCC07D213/74
Inventor 张治国颜吉校张富成
Owner 杭州瑞思新材料有限公司
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