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Synthesis method of benomyl

A synthetic method, the technology of benomyl, applied in the field of pesticides, can solve the problems of high cost, high price, and high safety risk, and achieve the effect of high safety and low cost

Inactive Publication Date: 2018-03-30
HUNAN GOFAR FINE CHEM IND TECH CO LDT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the low flash point and high price of methyl ethyl ketone, the safety risk in the production process is high, and the cost is also high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] At room temperature, 39 g of carbendazim (98%, 0.20 mol) and 156 g of dichloroethane were added to a 500 mL four-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and stirred for 15 min. Add 26 g (99%, 0.26 mol) of n-butyl isocyanate and stir for 15 min. Raise the temperature and keep the reaction at 75°C for 2h. Cool down, stir at 0°C for 30min, filter and dry. Benomyl 55.7g was obtained, with a content of 95.8% (91.9% yield), white.

Embodiment 2

[0023] At room temperature, 39 g of carbendazim (98%, 0.20 mol) and 195 g of dichloroethane were added to a 500 mL four-neck flask equipped with a stirrer, a thermometer and a reflux condenser, and stirred for 15 min. Add 26 g (99%, 0.26 mol) of n-butyl isocyanate and stir for 15 min. Raise the temperature and keep the reaction at 75°C for 2h. Cool down, stir at 0°C for 30min, filter and dry. Benomyl 55.9g was obtained, with a content of 95.8% (92.3% yield), white.

Embodiment 3

[0025] At room temperature, 39 g of carbendazim (98%, 0.20 mol) and 234 g of haloalkane were added to a 500 mL four-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and stirred for 15 min. Add 26 g (99%, 0.26 mol) of n-butyl isocyanate and stir for 15 min. Raise the temperature and keep the reaction at 75°C for 2h. Cool down, stir at 0°C for 30min, filter and dry. 55.8 g of benomyl was obtained, with a content of 95.7% (92.0% yield), white.

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PUM

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Abstract

The invention relates to a method for synthesizing benomyl, which comprises the following steps: 1) putting a certain amount of solvent and carbendazim into a reaction vessel at normal temperature, and stirring for 10-20 minutes, wherein the solvent is dichloroethane; 2) at normal temperature Put a certain amount of n-butyl isocyanate into the reaction vessel, and stir for 10-20 minutes after adding; 3) Raise the temperature, and keep it at 45°C~65°C for 2-4h; 4) Freeze, crystallize and filter the above-mentioned reacted materials , drying to obtain benomyl. The benomyl produced by the benomyl production process of the present invention has a white appearance, a content of more than 95.5%, high safety and low cost.

Description

technical field [0001] The invention relates to the field of pesticides, in particular to a synthesis method of the fungicide benomyl original drug. Background technique [0002] Benomyl is a systemic fungicide, which is effective against diseases caused by Ascomycetes, Deuteromycetes and some Basidiomycetes on cereal crops, grapes, pome fruits and stone fruits, rice and vegetables. It can also be used to prevent and control mites, has low toxicity to humans and animals, and is safe to crops. [0003] At present, butanone is used as solvent in the synthesis process of benomyl, and n-butyl isocyanate is added dropwise at high temperature, the reaction temperature is 70°C, the product content is between 94.5% and 95%, and the appearance is off-white or light yellow. Due to the low flash point and high price of methyl ethyl ketone, the safety risk in the production process is high, and the cost is also high. Contents of the invention [0004] The purpose of the present inve...

Claims

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Application Information

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IPC IPC(8): C07D235/32
CPCC07D235/32
Inventor 陈儒贵闾忠贤朱俊杰龚炳炎
Owner HUNAN GOFAR FINE CHEM IND TECH CO LDT
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