Synthesis process of trichloro pyridyl sodium alcoholate

A technology for the synthesis process of sodium clopyridinate, which is applied in the field of synthesis process of sodium clopyridinate, can solve the problems of increased difficulty in operation and control, complex refining process, and complicated production process, so as to save raw materials and improve the reaction rate. The effect of high yield and purity

Inactive Publication Date: 2007-08-22
BLUESTAR LEHIGH ENG INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The synthetic technique of existing triclopyridinate sodium mainly has the following disadvantages: (1) in order to prevent the occurrence of side reactions such as decomposition, the process needs nitrogen protection; (2) acrylonitrile and trichloroacetyl chloride generate 3 by addition and cyclization, 3,5,6-tetrachloro-3,4-dihydropyridin-2-one needs to supplement HCl gas during the ring closure process, so it needs to pressurize and feed HCl gas, which makes the production process complicated and the operation and control more difficult (3) At present, most of the refining process of the product at home and abroad adopts dissolving the product in water and heating to reflux to remove the solvent, and then the product is cooled and crystallized in water. Therefore, the product refining process is complicated and the waste water is much

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1. A kind of synthetic technique of triclopyridinate sodium, its step is as follows,

[0016] (1) Trichloroacetyl chloride, acrylonitrile, nitrobenzene and a catalyst made of cuprous chloride, copper powder and zinc powder are dropped into the reactor, wherein the mol ratio of trichloroacetyl chloride to acrylonitrile is 1: 1. The weight ratio of the catalyst cuprous chloride, copper powder and zinc powder is 1:0.2:0.2, heat up to 40°C, keep warm for 20 minutes, add HCl gas controlled release agent, heat up to 70°C and reflux for 6 hours, add 15 % NaOH was heated to 75°C, kept at reflux for 3 hours, cooled to 25°C and filtered to obtain a crude product;

[0017] (2) Recover the solvent from the filtrate under reduced pressure, put the obtained crude product into an internal circulation crystallizer filled with water, heat up to 40°C to refine and remove impurities, and the crystallized product is discharged together with the mother liquor through the underflow,...

Embodiment 2

[0019] Example 2. A kind of synthetic technique of triclopyridinate sodium, its step is as follows,

[0020] (1) Trichloroacetyl chloride, acrylonitrile, nitrobenzene and a catalyst made of cuprous chloride, copper powder and zinc powder are dropped into the reactor, wherein the mol ratio of trichloroacetyl chloride to acrylonitrile is 1: 1.6, the weight ratio of the catalyst cuprous chloride, copper powder and zinc powder is 1:1.8:1, heat up to 60°C, keep warm for 40 minutes, add HCl gas controlled release agent, heat up to 160°C and reflux for 10 hours, add 25 % NaOH was heated to 85°C, kept at reflux for 4 hours, cooled to 35°C and filtered to obtain a crude product;

[0021] (2) Recover the solvent from the filtrate under reduced pressure, put the obtained crude product into an internal circulation crystallizer filled with water, heat up to 70°C to refine and remove impurities, and the crystallized product is discharged together with the mother liquor through the underflo...

Embodiment 3

[0023] Example 3. A kind of synthetic technique of triclopyridinate sodium, its step is as follows,

[0024] (1) Trichloroacetyl chloride, acrylonitrile, nitrobenzene and a catalyst made of cuprous chloride, copper powder and zinc powder are dropped into the reactor, wherein the mol ratio of trichloroacetyl chloride to acrylonitrile is 1: 1.2, the weight ratio of catalyst cuprous chloride, copper powder and zinc powder is 1:1:0.6, heat up to 50°C, keep warm for 30 minutes, add HCl gas controlled release agent, heat up to 100°C and reflux for 8 hours, add 20 % NaOH was heated to 80°C, kept at reflux for 3.5 hours, cooled to 30°C and filtered to obtain a crude product;

[0025] (2) Recover the solvent from the filtrate under reduced pressure, put the obtained crude product into an internal circulation crystallizer filled with water, heat up to 60°C to refine and remove impurities, and the crystallized product is discharged together with the mother liquor through the underflow, ...

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PUM

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Abstract

The present invention is synthesis process of trichloro pyridyl sodium alcoholate. The synthesis process includes the following steps: reaction of trichloroacetyl chloride, acrylonitrile, nitrobenzene and catalyst in a reactor at 40 -60 deg.c for 20-40 min; adding HCl gas release controlling agent and refluxing at 70-160 deg.c for 6-10 hr; adding 15-25 % concentration NaOH solution, heating to 75-85 deg.c and refluxing for 3-4 hr; cooling to 25-35 deg.c and filtering to obtain coarse product; decompressing the filtrate to recover solvent, re-crystallizing the coarse product for purifying at 40-70 deg.c in a internally circular crystallizer; centrifugally separating the mother liquid and drying to obtain the product; and returning the mother liquid to the crystallizer for reuse. The present invention has high product quality, high yield, less wastes and low production cost.

Description

technical field [0001] The invention relates to a method for preparing sodium clopyridinate, in particular to a synthesis process of sodium clopyridinate. Background technique [0002] The synthetic technique of existing triclopyridinate sodium mainly has the following disadvantages: (1) in order to prevent the occurrence of side reactions such as decomposition, the process needs nitrogen protection; (2) acrylonitrile and trichloroacetyl chloride generate 3 by addition and cyclization, 3,5,6-tetrachloro-3,4-dihydropyridin-2-one needs to supplement HCl gas during the ring closure process, so it needs to pressurize and feed HCl gas, which makes the production process complicated and the operation and control more difficult (3) At present, most of the refining process of the product at home and abroad adopts that the product is dissolved in water and heated to reflux to remove the solvent, and then the product is cooled and crystallized in water. Therefore, the product refining...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/64
Inventor 任鑫智李学字魏春城赵焰李永华
Owner BLUESTAR LEHIGH ENG INST CO LTD
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