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Thiocyclam synthesis method

A synthetic method and insecticidal ring technology, applied in the field of pesticide synthesis, can solve problems such as difficult to handle, difficult to handle formaldehyde, complex salt, etc., and achieve the effect of reducing environmental protection pressure filtration and increasing yield

Inactive Publication Date: 2014-04-30
JIANGSU TIANRONG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] This process uses formaldehyde as a reaction protection agent, the formaldehyde in the generated wastewater is difficult to handle, and the salt produced is complex and difficult to handle

Method used

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  • Thiocyclam synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put 78 grams of 35% dimehypo aqueous solution and 250ml of toluene into a 500ml four-necked reaction bottle, stir and cool down to 0°C, start to add 63 grams of 15% sodium sulfide aqueous solution dropwise, and drop it in 3 hours. Keep warm for 3 hours, filter, wash the filter cake with a small amount of water to obtain sodium sulfite, remove the lower layer of water from the filtrate, wash the oil layer with water, and obtain the oil layer, heat up to 20°C, slowly add 10.1 grams of oxalic acid, then heat up to 40°C, keep warm for 1 hour, and cool Filter and dry the filter cake to obtain the insecticidal ring. , weight 31.4 grams, content 95.0%, molar yield 95.5%. Melting point: 125~128℃.

Embodiment 2

[0029] Put 78 grams of 35% dimehypo aqueous solution and 300ml of toluene into a 500ml four-necked reaction bottle, stir and cool down to 0°C, start to add 70 grams of 15% sodium sulfide aqueous solution dropwise, and drop it in 3 hours. Insulate for 3 hours, filter, wash the filter cake with a small amount of water to obtain sodium sulfite, separate the filtrate from the lower layer of water, wash the oil layer with water, and obtain the oil layer, raise the temperature to 20°C, slowly add 10.1 grams of oxalic acid, then raise the temperature to 50°C, keep it warm for 1 hour, and cool Filter and dry the filter cake to obtain the insecticidal ring. , weight 31.2 grams, content 95.0%, molar yield 95.1%.

Embodiment 3

[0031] Put 78 grams of 35% dimehypo aqueous solution and 300ml of toluene into a 500ml four-necked reaction bottle, stir and cool down to 0°C, start to add 65 grams of 15% sodium sulfide aqueous solution dropwise, and drop it in 3 hours. Keep warm at ℃ for 3 hours, filter, wash the filter cake with a small amount of water to obtain sodium sulfite, separate the filtrate to remove the lower layer of water, wash the oil layer with water, and obtain the oil layer, heat up to 20°C, slowly add 10.1 grams of oxalic acid, and then heat up to 40°C ~ 60°C, keep warm 1 hour, cool and filter, and dry the filter cake to obtain the insecticidal ring. , weight 31.5 grams, content 95.5%, molar yield 96%.

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Abstract

The invention discloses a thiocyclam synthesis method. The method comprises the steps of mixing a thiocyclam aqueous solution in a medium solvent, cooling to be below 0 DEG C, slowly adding a sodium sulfide aqueous solution, dropwise adding for 0.5-5 hours at temperature ranging from -15 DEG C to 5 DEG C, preserving heat for 0.5 5 hours, implementing cyclization reaction, and filtering after reaction; washing and drying a filter cake obtained after filtering to obtain sodium sulfite; filtering to obtain filtrate layers, washing with water, and removing water at the lower layer, heating an oil layer to 20-30 DEG C, slowly adding oxalic acid, heating to 40-60 DEG C, preserving heat for 0.5-2 hours, cooling, filtering, and drying the filter cake to obtain thiocyclam. The synthesis method disclosed by the invention can prepare thiocyclam of which the content is more than 95%, and yield is more than 95%.

Description

technical field [0001] The invention belongs to the field of pesticide synthesis, and in particular relates to a method for synthesizing pesticide insecticidal rings. Background technique [0002] Insecticidal ring is a selective insecticide, which has stomach poisoning, contact killing, and systemic effects, and can be transmitted to the top. The duration of control of Lepidoptera and Coleoptera pests is 7 to 14 days, and it can also control parasitic nematodes, such as Rice white-pointed nematode also has a certain control effect on rust and white ear disease of some crops. It can prevent and control three stem borers, rice leaf rollers, rice stem borers, rice thrips, leafhoppers, rice gall midges, planthoppers, green peach aphids, apple aphids, apple red spiders, pear star caterpillars, citrus leaf miners, Vegetable pests, etc. The English common name is thiocyclam-hydrogen-oxalate; the free base is thiocyclam (BSI; ISO, JMAF), the trade name is insecticidal ring; , N-...

Claims

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Application Information

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IPC IPC(8): C07D341/00
CPCC07D341/00
Inventor 许网保臧伟新魏明阳虞国新
Owner JIANGSU TIANRONG GROUP
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