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Method for preparing new type bactericide of iso-thiazolinone

A technology of methyl isothiazolone and bactericide, which is applied in the field of compound preparation, can solve problems such as unfavorable closed-loop reaction, difficult removal, and difficult recovery, and achieves the effects of reducing side reactions, improving yield, and being easy to recover.

Inactive Publication Date: 2010-01-13
HUBEI DAYA BIOLOGICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0024] 1. During the acylation reaction, excessive methylamine aqueous solution is used as an acylating agent, and the trace water in the reaction product is difficult to remove, which is very unfavorable to the next step of the ring closure reaction, resulting in a relatively low conversion rate and yield of the ring closure reaction. The yield is only 30-40%
[0025] 2. Using SO in the ring-closing reaction 2 Cl 2 or Cl 2 When the ring-closing reaction is carried out, the amount of chlorinating agent is too large, it is not easy to recycle, and the disadvantages of polluting the environment
[0026] In order to solve the above-mentioned problems that isothiazolinone fungicides exist, many researchers have been studying different preparation methods, but have not found an ideal method.

Method used

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  • Method for preparing new type bactericide of iso-thiazolinone
  • Method for preparing new type bactericide of iso-thiazolinone
  • Method for preparing new type bactericide of iso-thiazolinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Preparation of dimethyl disulfide dipropionate

[0039] Add 84 grams of sodium bicarbonate to 86 grams of methyl acrylate and stir, cool in an ice bath to 0-15 ° C, dropwise add 300 grams of sodium polysulfide solution with a concentration of 40%, and after the addition is complete, continue stirring at room temperature for 5 After 1 hour, the lower layer product was separated from the upper layer aqueous solution, 500 grams of saturated sodium sulfite solution was added to the product, heated and stirred at 50 ° C for 3 hours, the reaction product was separated from the water phase again, separated and purified to obtain 192 grams of dimethyl disulfide dipropionate , the yield is 81%;

[0040] (2) Preparation of N, N'-dimethyldithiodipropionamide

[0041] Add 700 ml of N,N-dimethylformamide solution of methylamine dropwise to 192 g of dimethyl disulfide dipropionate, the temperature of the addition is controlled at 0-5°C, and after the addition, the temperature is...

Embodiment 2

[0045] (1), the preparation of dimethyl disulfide dipropionate

[0046] Raw material addition is identical with embodiment 1.

[0047] Add sodium bicarbonate to methyl acrylate for stirring, cool in an ice bath to 0-15°C, add sodium polysulfide solution dropwise, after the dropwise addition is complete, continue to stir and react at room temperature for 3 hours, separate the lower layer product from the upper layer aqueous solution, and Sodium sulfite solution was added to the product, heated and stirred at 50° C. for 3 hours, the reaction product was separated from the water phase again, separated and purified to obtain dimethyl disulfide dipropionate; the amount of raw materials added was the same as in Example 1.

[0048] (2) Preparation of N, N'-dimethyldithiodipropionamide

[0049] Raw material addition is identical with embodiment 1.

[0050] Add the N,N-dimethylformamide solution of methylamine dropwise to dimethyl disulfide dipropionate, the dropping temperature is c...

Embodiment 3

[0055] (1), the preparation of dimethyl disulfide dipropionate

[0056] Raw material addition is identical with embodiment 1.

[0057] Add sodium bicarbonate to methyl acrylate for stirring, cool in an ice bath to 0-15°C, add sodium polysulfide solution dropwise, after the dropwise addition is complete, continue to stir and react at room temperature for 3 hours, separate the lower layer product from the upper layer aqueous solution, and Add sodium sulfite solution to the product, heat and stir at 50°C for 3 hours, separate the reaction product from the water phase again, separate and purify to obtain dimethyl disulfide dipropionate;

[0058] (2) Preparation of N, N'-dimethyldithiodipropionamide

[0059] Raw material addition is identical with embodiment 1.

[0060]Add the N,N-dimethylformamide solution of methylamine dropwise to dimethyl disulfide dipropionate, the dropping temperature is controlled at 0-5°C, and after the dropwise addition, keep the reaction at 20-25°C for ...

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Abstract

This invention relates to a method for preparing a novel bactericide isothiazolinone. The method comprises: (1) adding sodium polysulfide into methyl acrylate for reaction, separating the products, and purifying to obtain dimethyl dipropionate disulfide; (2) adding DMF solution of methylamine, acylating, separating the products, and purifying to obtain N,N'-dimethyl dipropionamide disulfide; (3) dissolving in 1,2-dichloroethane, microwave-irradiating for ring-closing reaction, separating the products, and purifying to obtain isothiazolinone. The method has such advantages as high yield, and little pollution.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a preparation method of a fungicide isothiazolinone. Background technique [0002] Kejunqiang is a bactericidal preservative developed by American ROHM&HASS company in 1975. It is a water-soluble liquid preservative and a high-efficiency broad-spectrum antibacterial agent. It can be kept for more than one year at room temperature and 6 months at 50°C. above. Because of its high-efficiency and broad-spectrum advantages, it is a very versatile fungicide. [0003] Kejunqiang (KATHON) is also a low toxicity preservative. Kathon (KATHON) is mainly used for cosmetic antisepsis, and can also be used as a preservative in the fields of papermaking, cooling circulating water, metal cutting fluid, paint and wood, etc. It is a product worthy of vigorous development, with high additional value value. KATHON fungicides are active ingredients with the following two ingredients: [0004...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D275/03
Inventor 熊洪录徐振明徐丹代兵
Owner HUBEI DAYA BIOLOGICAL TECH CO LTD