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N-hydroxymethyl isothiazolinone preparation method

A technology of hydroxymethylisothiazolinone and butoxymethacrylamide, which is applied in the field of preparation of N-methylolisothiazolinone, can solve the problem of high cost, low yield, N-methylolisothiazolinone There are many reaction steps of thiazolinone, etc., to achieve the effect of low cost, high yield and few reaction steps

Inactive Publication Date: 2004-11-10
OCEAN UNIV OF CHINA
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  • Abstract
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AI Technical Summary

Problems solved by technology

The preparation method of this N-hydroxymethylisothiazolinone has the disadvantages of many reaction steps, low yield and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0007] 1. Preparation of sodium polysulfide

[0008] Add 200ml of water, 26.4g of sulfur powder and 50.1g of sodium sulfide into a 400ml beaker, heat to boiling under stirring conditions, filter after cooling to obtain a red clear sodium polysulfide aqueous solution, cool to 0-5°C for later use.

[0009] 2. Preparation of dithiobis(N-dibutoxymethacrylamide)

[0010] In a 1000ml three-neck flask equipped with a stirring device, a condenser, and a thermometer, add 76.0 grams of N-butoxymethacrylamide, 60 grams of sodium bicarbonate, 500 ml of an aqueous solution, and 80 ml of ethanol, and control the reaction temperature at 0 to 5 ° C. The sodium polysulfide aqueous solution prepared above was added dropwise within 1.5 hours under stirring. Then react at room temperature for 5 to 6 hours to end the reaction. A yellow solid was obtained by suction filtration, to which 360ml (1mol / L) of sodium sulfite aqueous solution was added, stirred to obtain a white paste, the precipitate w...

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Abstract

A process for preparing N-methylol isothiazolinone comprises reacting N-butoxy methacrylamide with sodium polysulfide, creating 2 (N-butoxymethacrylic acid acidamide) disulfide, which is being subjected to reaction with sulfuric chloride to obtain N-methylol isothiazolinone, the reaction between N-butoxy methacrylamide and sodium polysulfide being carried in water and the solution of ethanol or methanol, the weight ratio of water and methanol or ethanol or propanol or butanol is 1:0.01-2.

Description

technical field [0001] The invention relates to an isothiazolinone, in particular to a preparation method of N-methylolisothiazolinone. Background technique [0002] The structural formula of isothiazolinone compound (Isothiazolone) is where the R 1 and R 2 Can be the same or different, they can all be H, halogen, C 1 -C 4 of alkyl. Y can be C 1 -C 8 Alkyl, C 3 -C 6 Cycloalkyl groups, aralkyl groups of up to 8 carbon atoms, aromatic hydrocarbon groups, or aromatic hydrocarbon groups of 6 carbon atoms with substituents. If Y in this formula is a lower alkane, then at least one R 1 or R 2 for H (generally R 1 for H). These compounds are a new type of high-efficiency broad-spectrum fungicides, which have the advantages of high efficiency, low toxicity, long duration of drug effect, and no harm to the environment. Therefore, it is widely used in industrial water treatment, cosmetics, building materials, adhesives, coatings, medical and health, textiles, photograph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D275/02
Inventor 于良民徐焕志张志明
Owner OCEAN UNIV OF CHINA