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Preparation method for iodopropynyl butylcarbamate

A technology for butyl propynyl carbamate and propargyl ester, which is applied in the field of broad-spectrum fungicide preparation, can solve the problems of high reaction cost, safety and environmental pollution, complicated reaction steps, etc. The effect of high rate and simple reaction steps

Inactive Publication Date: 2018-04-27
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This type of method has the following disadvantages: 1) the method adopts n-butyl isocyanate as the starting raw material, and the reaction cost is high, and the raw material is unstable and easy to decompose. 2) the method adopts dichloroketone as the starting raw material, and the reaction The conditions are harsh and unstable, and the cost is high, and the reaction steps are cumbersome. In the process of industrial mass production, a large amount of highly toxic cyanide is used. In the process of production and post-processing, if it is not handled properly, it will cause serious safety and environmental pollution. And other issues

Method used

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  • Preparation method for iodopropynyl butylcarbamate
  • Preparation method for iodopropynyl butylcarbamate

Examples

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Effect test

Embodiment 1

[0016] Embodiment 1 A kind of preparation method of iodopropynyl butyl carbamate

[0017] 1) Weigh 58kg of sodium bicarbonate and 68kg of propyne bromide and dissolve them in 150L of nitrobenzene, then add them to the three-port reactor, after the addition is complete, heat up to 120°C, and keep the dropwise reaction temperature at 120°C to 140°C, continue After the reaction was completed for 36 hours, the organic solvent was directly filtered and distilled under reduced pressure to obtain 50 kg of 1-hydroxyformic acid-3-propynyl ester, and the yield (calculated as propyne bromide) was 88%.

[0018] 2) Weigh 75kg of potassium bicarbonate and 43kg of propyne chloride, dissolve them in 150L of dimethylformamide, add them to the three-port reactor, and raise the temperature to 120°C after the addition, and keep the dropwise reaction temperature at 120°C to 140°C , continue the reaction for 48h, and after the reaction is completed, directly filter and distill the organic solvent u...

Embodiment 2

[0022] 1) Weigh 68kg of 1-hydroxyformic acid-3-propynyl ester and 45kg of 1-butylamine and dissolve it in 150L of dimethoxydimethyl ether, add it to the three-port reactor, and after the temperature drops to 0-5°C, Slowly add 16kg of concentrated hydrochloric acid solution, the temperature rises to 120°C after the addition, and the reaction time is 12h. After the reaction is completed and the temperature drops to 5-10°C, continue to add 11kg of sodium iodide, and the temperature is raised to 25-30°C after the addition, and the reaction is continued for 24h , the resulting reaction solution was distilled under reduced pressure to remove the solvent, added an excess of 800mL of water and stirred for 30 minutes, filtered, and dried to obtain 157kg, iodopropynyl butyl carbamate, and the yield (in terms of 1-butylamine) was 91 %.

[0023] 2) Weigh 60kg of 1-hydroxyformic acid-3-propynyl ester and 37kg of 1-butylamine, dissolve them in 150L of diisopropyl ether, and add them into th...

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Abstract

The invention discloses a preparation method for iodopropynyl butylcarbamate, belonging to the technical field of preparation technology for wide-spectrum bactericides. The preparation method comprises the following steps: dissolving bicarbonate and halogen propyne in an organic solvent, carrying out a reaction under a reflux condition so as to obtain 1-hydroxy-3-propyne formate, and subjecting 1-hydroxy-3-propyne formate to acid dehydration and iodine oxidation so as to directly prepare the final product iodopropynyl butylcarbamate. The preparation method uses cheap and easily available raw materials, is simple in reaction steps, high in yield, almost free of pollution, free of harsh and dangerous reaction conditions and suitable for domestic mass production, and the prepared iodopropynylbutylcarbamate is easy to purify.

Description

technical field [0001] The invention belongs to the technical field of preparation of broad-spectrum fungicides, in particular to a preparation method of iodopropynyl butyl carbamate Background technique [0002] Iodo-propynyl butylcarbamate (3-Iodo-2-propynyl butylcarbamate, IPBC) was mainly used in coatings, paints, wood preservatives, skin care and cosmetics in the 1970s, and is used globally for water-soluble antiseptics agent. As a broad-spectrum bactericide, IPBC can effectively kill mold, yeast, algae and bacteria, and has special effects on fungi; it has low toxicity, high activity and other effects, and it is also widely used in the field of microorganisms. [0003] The past synthetic method of butyl iodopropynyl carbamate mainly uses two kinds of methods 1) n-butyl isocyanate and propynyl alcohol react under alkaline conditions, then add iodine again and make; 2) propynyl alcohol It reacts with dichloroketone, then adds butylamine again to obtain amide, and final...

Claims

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Application Information

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IPC IPC(8): C07C269/04C07C271/12
CPCC07C68/00C07C269/04C07C271/12C07C69/96
Inventor 金国范
Owner JIANGSU UNIV
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