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Industrialized method for preparing 2-mercaptopyridine

A technology of mercaptopyridine and chloropyridine, applied in the field of organic chemical synthesis, can solve the problems of high price, long synthesis steps, harsh conditions, etc., and achieves the effects of solving industrialized production problems, simple and convenient production process, and mild reaction conditions

Inactive Publication Date: 2011-01-12
TIANJIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of 2-mercaptopyridine uses expensive starting material pyridine raw materials, and the synthesis steps are longer, the conditions of key reactions are harsh, and the overall reaction yield is low, which makes 2-mercaptopyridine and its nitrogen The price of metal salts of oxides has remained high for a long time, and it has even been out of stock for a long time in China
[0006] The above two methods have problems such as expensive raw materials or long reaction steps or low yields
At present, there are few reports and applications for the preparation of 2-mercaptopyridine patents, and there is no literature report on the one-step method for preparing 2-mercaptopyridine.

Method used

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  • Industrialized method for preparing 2-mercaptopyridine
  • Industrialized method for preparing 2-mercaptopyridine
  • Industrialized method for preparing 2-mercaptopyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 135kg of anhydrous sodium hydrosulfide (with a content above 99%) and 300kg of ethylene glycol into a conical reaction kettle equipped with a stirrer, a thermometer, a reflux device, a distillation device, a heating device and a feeding device, start stirring, and close the distillation device, open the reflux device, heat to 120°C, add 60kg of 2-chloropyridine to the feeding port, after 2 hours, add 60kg of 2-chloropyridine for the second time, and after another 2 hours, add 60kg of 2-chloropyridine for the third time Pyridine, after 2 hours, add 50kg2-chloropyridine again, add 230kg altogether, 2-chloropyridine, react after 18 hours, open distillation device, close reflux device, distill off solvent, add 200kg distilled water, temperature is down to room temperature, use dilute Adjust the pH value to 6-7 with hydrochloric acid, crystals are precipitated, add chloroform for extraction, use 100kg chloroform for extraction each time, extract three times in total, coll...

Embodiment 2

[0027] Anhydrous sodium hydrosulfide (content is more than 99%) 160kg and 400kg propylene glycol are joined in the conical reaction kettle that stirrer, thermometer, reflux device, distillation unit, heating unit feeding device are housed, start stirring, close distillation unit, Open the reflux device, heat to 160°C, add 60kg 2-chloropyridine at the feed port, after 2 hours, add 60kg, 2-chloropyridine for the second time, and after 2 hours, add 60kg, 2-chloropyridine for the third time, After 2 hours, add 50kg again, 2-chloropyridine, add 230kg altogether, 2-chloropyridine, react after 12 hours, open distillation device, close reflux device, distill off solvent, add 200kg distilled water, temperature is down to room temperature, use dilute Adjust the pH value to 5 with hydrochloric acid, crystals are precipitated, add toluene for extraction, use 100kg of toluene each time for extraction, and extract three times in total, collect the extract to the distillation pot, distill and...

Embodiment 3

[0029] Add 170kg of anhydrous sodium hydrosulfide (content above 99%), 400kg of mixed solution of cyclohexanol and ethylene glycol (mass ratio is 1:1) to the tank equipped with agitator, thermometer, reflux device, distillation device and heating device. In the conical reactor of the feeding device, start stirring, close the distillation device, open the reflux device, heat to 120°C, add 60kg of 2-chloropyridine to the feeding port, and after 2 hours, add 60kg of 2-chloropyridine for the second time After 2 hours, add 60kg, 2-chloropyridine for the third time, after 2 hours, add 50kg, 2-chloropyridine, add 230kg, 2-chloropyridine altogether, after reacting for 14 hours, open the distillation unit, close the reflux device, remove the solvent by distillation, add 250kg of distilled water, adjust the pH value to 6-7 with dilute acetic acid, crystals are precipitated, add toluene for extraction, use 100kg of toluene each time for extraction, and extract three times in total, collec...

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Abstract

The invention discloses an industrialized method for preparing 2-mercaptopyridine, which comprises the following production processes of: adding anhydrous sodium bisulfide and an organic solvent into a conical reactor with a stirrer, a thermometer, a reflux device, a distilling device, a heating device and a charging device, heating to a certain temperature, adding 2-chloropyridine in batches from a charging opening, performing reaction for several hours until the reaction is completed, removing a solvent by distilling, adding an appropriate amount of distilled water, regulating the pH value by using acid, extracting by using the organic solvent, and removing an extracting agent by distilling to obtain faint yellow 2-mercaptopyridine crystals. The preparation method of the invention has the advantages of simple and convenient production process, mild reaction conditions, and high yield and purity of products; and the industrialized method for synthesizing the 2-mercaptopyridine in one step is provided and the problem of industrialized production of the 2-mercaptopyridine is solved.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and relates to an industrialized method for preparing 2-mercaptopyridine, in particular to the industrialization of preparing 2-mercaptopyridine in one-step method by heating with an appropriate solvent using industrial anhydrous sodium hydrosulfide and 2-chloropyridine as raw materials method. Background technique [0002] 2-Mercaptopyridine is a kind of fine chemicals and pharmaceutical intermediates widely used in organic synthesis and industrial production. The preparation of 2-mercaptopyridine uses expensive starting material pyridine raw materials, and the synthesis steps are longer, the conditions of key reactions are harsh, and the overall reaction yield is low, which makes 2-mercaptopyridine and its nitrogen The price of metal salts of oxides has remained high for a long time, and they have even been out of stock for a long time in China. Therefore, the key to studyi...

Claims

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Application Information

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IPC IPC(8): C07D213/70
Inventor 刘尚远赵小军尹振明王倩
Owner TIANJIN NORMAL UNIVERSITY
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