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Preparation method of bendiocarb intermediate and active ingredient

A technology of dicarbacarb and intermediates, which is applied in the field of preparation of dicarbacarb technical materials, can solve the problems of equipment design and industrial application difficulties, long operation time, long reaction time, etc., and achieve shortened reaction time, simple processing, and high reaction time. The effect of improving efficiency

Inactive Publication Date: 2019-07-26
SHANDONG WEIFANG RAINBOW CHEM
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  • Abstract
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AI Technical Summary

Problems solved by technology

However, since the boiling point of the by-product 2-methoxypropene is 34-36°C, which is lower than the boiling point of methanol, it is easier to evaporate out of the system than methanol and cause losses. Therefore, this method has difficulties in equipment design and industrial application. In addition, the operation time of the modified method long
[0005] U.S. Patent No. 3969416 first uses toluene or xylene as a solvent to react pyrogallic acid and 2,2-dimethoxypropane to generate 4-hydroxy-2,3-dimethyl-1,3-benzodioxol, However, the distilled light components need to be treated under the catalysis of sulfonic acid ion exchange resin, which is cumbersome to operate; and the single-step yield of dicarbacarb is only 86%, the reaction time is long and the yield is low

Method used

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  • Preparation method of bendiocarb intermediate and active ingredient
  • Preparation method of bendiocarb intermediate and active ingredient

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032]360ml of xylene, 84g (0.659mol) of pyrogallic acid and 101g (0.962mol) of 2,2-di Methoxypropane, dissolve 176g (1.673mol) 2,2-dimethoxypropane in 100ml xylene, put the 2,2-dimethoxypropane solution in a constant pressure funnel, and gradually Raise the temperature, control the reaction temperature to 102°C and carry out the reaction for 1-1.5 hours, while distilling off the light components; Evaporate the light components while adding dropwise. After about 4-5 hours, the dropwise addition is completed, and the light components collected in the water separator are released continuously, so as not to form reflux. When it is detected that the unconverted rate of pyrogallic acid is less than 2.2wt%, the reaction solution is cooled to obtain 595.1g intermediate 2,2-dimethyl-4-hydroxyl-1,3-benzodioxol feed solution, The content is 17.5wt%, and the yield is 95.1% based on pyrogallic acid. Add 50g of 14wt% sodium hydroxide solution to the distilled light component, stir and wa...

Embodiment 2

[0035] 300ml of xylene, 84g (0.659mol) of pyrogallic acid and 81g (0.769mol) of 2,2-di For methoxypropane, dissolve 222.5g (2.115mol) 2,2-dimethoxypropane in 120ml xylene, fill the 2,2-dimethoxypropane solution in a constant pressure funnel, and stir under magnetic force Gradually raise the temperature, control the reaction temperature to 102°C for 1-1.5 hours, and distill off the light components at the same time; Evaporate the light components while adding dropwise. After about 4.5 hours, the dropwise addition is completed, and the light components collected in the water separator are released continuously, so as not to form reflux. When it is detected that the unconverted rate of pyrogallic acid is less than 2.2wt%, the reaction is stopped, and the temperature is lowered to obtain 617.3g of intermediate 2,2-dimethyl-4-hydroxyl-1,3-benzodioxol feed solution, the content It is 16.8wt%, and the yield is 94.7% based on pyrogallic acid. Add 50g of 10wt% sodium hydroxide soluti...

Embodiment 3

[0038] Put 500ml xylene, 84g (0.659mol) pyrogallic acid and 141.6g (1.346mol) 2,2 - Dimethoxypropane, dissolve 151.7g (1.442mol) 2,2-dimethoxypropane in 90ml xylene, put the 2,2-dimethoxypropane solution in a constant pressure funnel, and stir it magnetically Gradually raise the temperature, control the reaction temperature to 102°C for 1-1.5 hours, and distill off the light components at the same time; when the methanol no longer comes out, drop the 2,2-dimethoxypropane solution in the constant pressure dropping funnel, Evaporate the light components while adding dropwise. After the dropwise addition is completed in about 5 hours, the light components collected in the water separator are continuously released to prevent reflux. When it is detected that the unconverted rate of pyrogallic acid is less than 2.2wt%, the reaction is stopped, and the temperature is lowered to obtain 627.3g of intermediate 2,2-dimethyl-4-hydroxyl-1,3-benzodioxol feed solution. It is 16.5wt%, and th...

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Abstract

The invention discloses a preparation method of a bendiocarb intermediate and an active ingredient. The preparation method includes: allowing pyrogallic acid to react with 2, 2-dimethoxypropane to generate a 2, 2-dimethyl-4-hydroxyl-1, 3-benzodioxoles solution, and directly using light components 2, 2-dimethoxypropane, 2-methoxypropene and methanol which are evaporated out for next batch after alkali washing; allowing the 2, 2-dimethyl-4-hydroxyl-1, 3-benzodioxoles solution to react with methyl isocyanate to obtain the bendiocarb active ingredient. By recycling raw materials and byproducts, cost is lowered, operation is simplified, production efficiency is improved, and convenience is brought for industrial production.

Description

technical field [0001] The invention relates to a method for preparing a bentacarb original drug, in particular to a method for preparing a bentacarb original drug with simple operation and low raw material consumption, and belongs to the technical field of pesticide preparation. Background technique [0002] Dicarbacarb is a carbamate heterocyclic insecticide for both sanitation and agricultural production, chemical name: O-(2,2-dimethyl-1,3-benzodioxol)-4 -Methyl carbamate, trade name Fica (sanitary use), Garvox, Seedox (agricultural use), high guard, the structural formula is . Dicarbocarb is a high-efficiency, low-residue pesticide variety, which is in line with the national industrial policy on pesticide development. It is also a pesticide variety approved and promoted by the World Health Organization. It can achieve good control effects in hygiene and crop pests, and can It is used to control more than 300 kinds of soil and ground pests of more than 40 crops such as...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/46
CPCC07D317/46
Inventor 孙国庆侯永生徐高飞李海华李洪力
Owner SHANDONG WEIFANG RAINBOW CHEM
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