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Synthesis method for high-quality and low-cost bispyrithione

A bipyridinethione and synthesis method technology, which is applied in the field of bispyridinethione synthesis, can solve the problems of unreported target product quality, increased production cost, and restricted product quality, achieving stable and reliable quality, reduced cost of finished products, The effect of reducing the discharge of three wastes

Inactive Publication Date: 2013-01-16
BINHAI COUNTY MINGHONG FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned two synthetic methods that have been publicly reported have a single-step yield of more than 90%, but there is no report on the quality of the target product
Moreover, if it is necessary to react in an organic solvent, 2-mercaptopyridine-N-oxide must be anhydrously treated. When 2-mercaptopyridine-N-oxide encounters high temperature, it will decompose and denature under light, which seriously restricts the feasibility of this industrial operation. Sexuality, which leads to a rapid increase in production costs and also restricts product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1. Put 600g of 2-chloropyridine, 100g of maleic anhydride, 600g of hydrogen peroxide (35%) into a 5000ml four-necked flask, and start stirring and heat up to 60°C for 12 hours of continuous reaction to obtain 2-chloropyridine-N-oxide aqueous solution.

[0021] 2. Use 4000g of 2-chloromethane to extract the obtained 2-chloropyridine-N-oxide aqueous solution four times, combine the extraction phases, concentrate and crystallize, and obtain pure 2-chloropyridine-N-oxide.

[0022] 3. Put the purified 2-chloropyridine-N-oxide, 430g sodium sulfide, and 2000g high-purity water into a 5000ml four-neck flask in turn, start stirring, and heat up to 70°C. Add a part of sodium carbonate in time as the reaction progresses , adjust the pH of the system to be stable at 9 to 10, heat at 70°C for 2 hours after the reaction, and cool down after the heat preservation. An aqueous solution of sodium 2-mercaptopyridine-N-oxide was prepared.

[0023] 4. Use an appropriate amount of dilute s...

Embodiment 2

[0026] 1. Put 835g of 2-bromopyridine, 30g of sodium tungstate, and 600g of hydrogen peroxide (35%) into a 5000ml four-necked flask in sequence, start stirring and raise the temperature to 80°C for 10 hours of continuous reaction to prepare 2-chloropyridine-N-oxide aqueous solution.

[0027] 2. Use 6000gl, 2-dichloroethane to extract the obtained 2-chloropyridine-N-oxide aqueous solution four times, combine the extract phases, concentrate and crystallize, and obtain pure 2-chloropyridine-N-oxide.

[0028] 3. Put the purified 2-bromopyridine-N-oxide, 1200g sodium hydrosulfide (38%), and 1500g high-purity water into a 5000ml four-necked flask in turn, start stirring, and heat up to 80°C. Add a part of sodium hydroxide to adjust the pH of the system to be stable at 9 to 10. After the reaction is completed, keep the temperature at 80° C. for 2 hours, and cool down after the heat preservation. An aqueous solution of sodium 2-mercaptopyridine-N-oxide was prepared.

[0029] 4. Use a...

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Abstract

The invention discloses a synthesis method for synthesizing high-quality and low-cost bispyrithione and relates to a synthesis method for the bispyrithione. The synthesis method comprises the following steps of: 1, performing mild oxidation reaction on halogenated pyridine and hydrogen peroxide in the presence of a catalyst to synthesize halogenated pyridine-N-oxide; 2, extracting and purifying the halogenated pyridine-N-oxide by using a solvent; 3, reacting the purified halogenated pyridine-N-oxide and a sulfhydrylation reagent under the alkaline condition to obtain 2-mercaptopyridine-N-oxide sodium; reacting 4,2-mercaptopyridine-N-oxide sodium under the acid condition to obtain 2-mercaptopyridine-N-oxide; and reacting 5,2-mercaptopyridine-N-oxide and oxidant to obtain a targeted product bispyrithione. By the method, the quality stability of a product can reach more than 99.5 percent; reaction conditions are mild; and cost is low.

Description

Technical field: [0001] The invention relates to a method for synthesizing bispyridinethione, in particular to a method for synthesizing bispyridinethione with high quality and low metal ion sensitivity. Background technique: [0002] Bipyridinethione (BPT) is an excellent anti-dandruff and antipruritic agent with broad-spectrum antibacterial properties. It is widely used in transparent plastics, pharmaceutical intermediates and other fields. It has a certain solubility in water and can be used in transparent shampoo systems Medium, without affecting the pearlescent effect of the shampoo system. Due to its unique molecular structure (the structural formula is as follows:) compared with the traditional anti-dandruff agent zinc pyrithione (ZPT), it greatly reduces its sensitivity to metal ions and exists more stably in the shampoo system. [0003] At present, there are no domestic and foreign reports on the route of synthesizing bispyridinethione from halogenated pyridines. T...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/89
Inventor 陈锋赵忠勇石峻冯启华冯启明李传峰郑兆金吴永平
Owner BINHAI COUNTY MINGHONG FINE CHEM
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