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Synthesis method of zinc pyrithione

A technique for zinc pyrithione and a synthesis method, applied in the direction of organic chemistry, can solve the problems of difficult purification, low product content, poor color of zinc pyrithione, etc., achieve reduction of sulfate content, simple process operation, and reduction of Effect of Salt Content

Inactive Publication Date: 2018-01-26
JIANGSU ZHONGBANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, either method does not produce products with high
Zinc pyrithione is an organometallic salt, which is insoluble in conventional solvents, making it difficult to purify and refine. Patent CN102603625B discloses a new method for purifying zinc pyrithione, but the color of zinc pyrithione obtained by this method is different from that of the phase before refining. Relatively poor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 20g 2-chloropyridine and 0.6g catalyst TiO in the 500ml reaction bottle 2 , heated up to 50°C, added dropwise 20g of 30% hydrogen peroxide, the amount of hydrogen peroxide and 2-chloropyridine in a ratio of 1:1, reacted for 10 hours, lowered to normal temperature, filtered, and the filter cake was drained , washed with 10g of deionized water, and the filtrate was 2-chloropyridine nitrogen oxide aqueous solution; the temperature of the system was raised to 70°C, and the mixture was added dropwise to 30g of 25% NaOH solution and 21g of 43% NaHS solution, and kept for 6 hours. Then cool down to room temperature, adjust the pH value to 4.5, add 1g of activated carbon for decolorization for 0.5h, and obtain a 2-mercaptopyridine-N-oxide solution; add 7.2g of zinc oxide to the 2-mercaptopyridine-N-oxide solution, and react at 70°C 6h, filtered, washed with water, and dried to obtain zinc pyrithione. Yield 94.3%, content 99.1%.

Embodiment 2

[0036] Add 20g 2-chloropyridine and 1.2g catalyst TiO in the 500ml reaction bottle 2 , heated up to 70°C, added dropwise 30g of 30% hydrogen peroxide, the amount of hydrogen peroxide and 2-chloropyridine in a ratio of 1.5:1, reacted for 4 hours, lowered to normal temperature, filtered, and the filter cake was drained , washed with 10g deionized water, and the filtrate was 2-chloropyridine nitrogen oxide aqueous solution; the system was heated to 80°C, and added dropwise to a mixture of 30g 25% NaOH solution and 24g 43% NaHS solution, and kept for 4 hours. Then cool down to room temperature, adjust the pH to 5, add 1.5g of activated carbon for decolorization for 0.5h, and obtain a 2-mercaptopyridine-N-oxide solution; add 7.2g of zinc oxide to the 2-mercaptopyridine-N-oxide solution, and heat React for 4 hours, filter, wash with water, and dry to obtain zinc pyrithione. Yield 92.7%, content 99.3%.

Embodiment 3

[0038] Add 20g 2-chloropyridine and 1.8g catalyst TiO in the 500ml reaction bottle 2 , heated up to 90°C, added dropwise 40g of 30% hydrogen peroxide, the amount of hydrogen peroxide and 2-chloropyridine in a ratio of 2:1, reacted for 3 hours, dropped to normal temperature, filtered, and the filter cake was drained , washed with 10g of deionized water, and the filtrate was 2-chloropyridine nitrogen oxide aqueous solution; the system was heated to 90°C, and added dropwise to a mixture of 30g of 25% NaOH solution and 27g of 43% NaHS solution, and kept for 2 hours. Then cool down to room temperature, adjust the pH value to 6, add 2g of activated carbon for decolorization for 0.5h, and obtain a 2-mercaptopyridine-N-oxide solution; add 7.2g of zinc oxide to the 2-mercaptopyridine-N-oxide solution, and react at 90°C 3h, filtered, washed with water, and dried to obtain zinc pyrithione. Yield 92.4%, content 99.2%.

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Abstract

The invention discloses a synthesis method of zinc pyrithione, and belongs to the field of organic synthesis. According to the synthesis method, 2-chloropyridine is used as a raw material; a final product is obtained through three steps of reactions of nitrogen oxidation, sulfhydrylation and salt formation. The synthesis method is simple in step and convenient to operate and further, the content of an obtained product is high.

Description

Technical field: [0001] The invention relates to a method for synthesizing zinc pyrithione, which belongs to the field of pharmaceutical manufacturing. Background technique: [0002] Zinc pyrithione, also known as zinc omadine (ZPT), has a molecular formula of C 10 h 8 N 2 o 2 S 2 Zn, a milky white aqueous dispersion or off-white powdery solid. [0003] Zinc pyrithione is used in shampoos to remove dandruff, and can inhibit the growth of Gram-positive and negative bacteria and molds. It can effectively care for hair, delay the aging of hair, and control the occurrence of gray hair and hair loss. In addition, it is also used as a cosmetic preservative, oil agent, and paint biocide. It can also be used as a preservative, antifouling agent, etc., and is widely used in fields such as agriculture, industry, medicine and hygiene, and cosmetics. [0004] There are many existing synthetic techniques for zinc pyrithione, which can generally be divided into three types: ① usin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/89
Inventor 吴四清蒋海松王红喜吴小刚钱勇徐强
Owner JIANGSU ZHONGBANG PHARMA
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