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Method for synthesizing thiacloprid active compound and co-producing carbon powder

A technology of thiacloprid and carbon powder, which is applied in the preparation/purification of carbon, organic chemistry and other directions, can solve problems such as high price and achieve good environmental benefits

Inactive Publication Date: 2013-06-12
葛瑞武
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the various production methods commonly used at present all need to use expensive and easy-to-polymerize cyanamide as a raw material, and need to add liquid caustic soda and other phase transfer catalysts

Method used

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  • Method for synthesizing thiacloprid active compound and co-producing carbon powder
  • Method for synthesizing thiacloprid active compound and co-producing carbon powder
  • Method for synthesizing thiacloprid active compound and co-producing carbon powder

Examples

Experimental program
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Effect test

Embodiment 1

[0023] 1. Synthesis of dimethyl dicarboxylate:

[0024] Add 300ml of water and 100g of lime nitrogen into a 1000ml three-necked bottle, control the temperature at 15°C, and add 90g of CS dropwise within one hour at a stirring speed of 90 rpm. 2 , after the dropwise addition was completed, the temperature began to rise to 42°C until CS 2 No more reflux. After filtering the solution in the bottle (collecting the filter cake for recycling carbon powder), the filtrate was added dropwise in an ice-water bath (CH 3 ) 2 SO 4 300g, adjust the dropping speed, and control the temperature below 10°C. After the dropwise addition, raise the temperature to 25°C and stir (90 rpm) for 4 hours, then cool down to 10°C to crystallize, and filter to obtain 105g of crude product .

[0025] 2. Preparation of thiazolidine:

[0026] Add 300ml of water to the there-necked flask, then add 15g of sodium hydroxide, stir to dissolve, cool down to 8°C, quickly add 60g of cysteamine hydrochloride, sti...

Embodiment 2

[0030] Add 500ml of water and 250g of lime nitrogen into a 1000ml three-necked bottle, control the temperature at 15°C, and add 135g of CS dropwise within one hour while stirring 2 , after the dropwise addition is completed, start to heat up to 42°C until CS 2 No more reflux. After filtering the solution in the bottle (collecting the filter cake for recycling carbon powder), the filtrate was added dropwise in an ice-water bath (CH 3 ) 2 SO 4 400 grams, adjust the dropping speed, control the temperature below 10°C, after the dropwise addition is complete, raise the temperature to 25°C and stir for 6 hours, then allow it to cool down and crystallize, and filter to obtain 201g of the crude product.

[0031] Add 600ml of water to the there-necked flask, then add 36g of sodium hydroxide, stir to dissolve, cool down to 8°C, quickly add 112g of cysteamine hydrochloride, stir to dissolve, add 140g of dimethyl dicarboxylate, stir for 40 minutes HPLC Detection, when the liquid phase...

Embodiment 3

[0035] Add 1260ml of water and 400g of lime nitrogen into a 2000ml three-necked bottle, control the temperature at 5-20°C, add 216g of CS dropwise within one hour under stirring 2 , after the dropwise addition is completed, start to heat up to 40-43°C until CS 2 No more reflux. After filtering the solution in the bottle (collecting the filter cake for recycling carbon powder), the filtrate was added dropwise in an ice-water bath (CH 3 ) 2 SO 4 540 grams, adjust the dropping speed, control the temperature below 10°C, after the dropwise addition is completed, heat up to 25°C and stir for 5 hours, then allow it to cool down and crystallize, and filter to obtain 400g of crude product.

[0036]Add 1200ml of water to the three-necked flask, then add 60g of sodium hydroxide, stir to dissolve, then cool down to 8°C, quickly add 200g of cysteamine hydrochloride, stir to dissolve, add 250g of dimethyl dicarboxylate, stir for 40 minutes HPLC Detection, when the liquid phase content o...

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Abstract

The invention relates to a preparation method of a chlorinated neonicotinoid insecticide and particularly relates to a method for synthesizing a thiacloprid active compound and co-producing carbon powder. The method is characterized by including the steps of putting water with the weight being 3-6 times that of lime nitrogen into a reaction kettle, adding lime nitrogen powder under the condition of stirring, dropwise adding carbon disulfide with the weight being 30-80% of that of the lime nitrogen at 5-20 DEG C after the completion of adding, continuously stirring at 30-43 DEG C until carbon disulfide backflow does not exist in the reaction kettle after the completion of dropwise adding, then carrying out thermal filtration, and collecting a filter cake and filtrate respectively. The method provided by the invention avoids the use of cyanamide which is high in cost and easy to aggregate as a raw material, uses the lime nitrogen which is cheap and easy to obtain for replacing the cyanamide, and recycles slag, thus providing an industrial synthesis way of the thiacloprid active compound which is green and economical, and has good environmental benefits.

Description

technical field [0001] The invention relates to a preparation method of chloronicotinoid insecticides, in particular to a method for synthesizing the original drug of thiacloprid and co-producing carbon powder. Background technique [0002] Thiacloprid is a new type of chloronicotinoid insecticide developed jointly by Bayer Agrochemical Company of Germany and Bayer Agrochemical Company of Japan. Its mechanism of action is different from other traditional insecticides. It mainly acts on the post-junction membrane of insect nerves. By combining with nicotinic acetylcholine receptors, it interferes with the normal conduction of the insect nervous system, causing blockage of nerve channels, resulting in a large accumulation of acetylcholine, which makes insects extremely excited, body convulsions, paralysis and death. . It has strong systemic, contact and stomach poisoning effects, and has no cross-resistance with conventional insecticides such as pyrethroids, organophosphorus...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D417/06C01B31/02C01B32/05
Inventor 杨文茂葛瑞武王邵贤
Owner 葛瑞武
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