A kind of preparation method of decinil

A technology of desiginil and molar ratio, which is applied in the field of preparation of desiginil, can solve the problems of toxicity of synthetic raw materials, high requirements for synthesis conditions, low reaction yield and the like, and achieves high purity, high yield, and operation steps. simple effect

Active Publication Date: 2016-12-07
QILU SYNVA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems of high requirements on synthetic conditions, high toxicity of synthetic raw materials and low reaction yield in the existing production process of decinil, the invention provides a preparation method of decinil

Method used

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  • A kind of preparation method of decinil

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Effect test

Embodiment 1

[0026] A preparation method of decinil, the steps are as follows:

[0027] 1) Put 100kg of guanidine hydrochloride and 114kg of bromocyclopropane into 600kg of acetone, stir evenly, add 144kg of potassium carbonate, heat up to 30°C, react for 2.0h, cool down to room temperature, filter, and concentrate the filtrate to dryness under reduced pressure to prepare Obtain intermediate 193.4kg, molar yield 90%;

[0028] 2) Add 374kg of purified water to 193.4kg of the intermediate obtained in step 1), stir evenly, add 90.5kg of 2-fluoromalonamide and 231kg ​​of 20% sulfuric acid, raise the temperature of the system to 30°C, react for 4.0h, and drop to At room temperature, adjust the pH of the system to 7.0 with sodium hydroxide solution, continue to stir, filter, and wash the filter cake with a large amount of water to obtain 112kg of 4,6-diamino-5-fluoro-2-cyclopropylaminopyrimidine, with a yield of 65 %;

[0029] 3) Dissolve 112kg of the prepared 4,6-diamino-5-fluoro-2-cyclopropy...

Embodiment 2

[0032] A preparation method of decinil, the steps are as follows:

[0033] 1) Put 100kg of guanidine hydrochloride and 253kg of bromocyclopropane into 1000kg of acetone, stir evenly, add 289kg of potassium carbonate, heat up to 80°C, react for 4.0h, cool down to room temperature, filter, and concentrate the filtrate to dryness under reduced pressure to prepare Obtain intermediate 195.4kg, molar yield 92%;

[0034] 2) Add 592kg of purified water to 195.4kg of the intermediate obtained in step 1), stir well, add 238.8kg of 2-fluoromalonamide, 487kg of 20% sulfuric acid, raise the temperature of the system to 100°C, react for 5.0h, and drop to At room temperature, adjust the pH of the system to 10.0 with sodium hydroxide solution, continue to stir, filter, and rinse the filter cake with a large amount of water to obtain 118kg of 4,6-diamino-5-fluoro-2-cyclopropylaminopyrimidine, with a molar yield of 67%;

[0035] 3) Dissolve 118kg of the prepared 4,6-diamino-5-fluoro-2-cyclopr...

Embodiment 3

[0038] A preparation method of decinil, the steps are as follows:

[0039] 1) Put 100kg of guanidine hydrochloride and 126.6kg of bromocyclopropane into 800kg of acetone, stir evenly, add 174.6kg of potassium carbonate, heat up to 50°C, react for 3.5h, cool down to room temperature, filter, and concentrate the filtrate to dryness under reduced pressure , obtained intermediate 198.6kg, molar yield 95%;

[0040] 2) Add 428kg of purified water to 198.6kg of the intermediate obtained in step 1), stir well, add 100.8kg of 2-fluoromalonamide, 305kg of 20% sulfuric acid, raise the temperature of the system to 80°C, and react for 4.0-5.0h, Cool down to room temperature, adjust the pH of the system to 7.5 with sodium hydroxide solution, continue to stir, filter, and rinse the filter cake with a large amount of water to obtain 123.9 kg of 4,6-diamino-5-fluoro-2-cyclopropylaminopyrimidine, The molar yield is 68%;

[0041] 3) Dissolve 123.9kg of the prepared 4,6-diamino-5-fluoro-2-cyclo...

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Abstract

The invention discloses a preparation method of dicyclanil, belongs to the field of preparation of growth regulators, and solves the problem that the existing dicyclanil production process is high in synthetic condition, great in toxicity of synthetic raw materials and low in reaction yield. The preparation method comprises the following steps: carrying out substitution reaction on guanidine hydrochloride and bromocyclopropane; carrying out closed-ring reaction on the product obtained from the former step and 2-fluoropropiondiamide; and finally substituting florine on aromatic rings by providing cyan groups from potassium ferrocyanide to obtain a dicyclanil product. The preparation method disclosed by the invention is simple in operating step, low in price of materials and high in yield, and the obtained product is high in purity and shallow in color, and dicyanomethane which is relatively great in toxicity is not used in the production process.

Description

technical field [0001] The invention relates to the technical field of insect growth regulators, in particular to a preparation method of decinil. Background technique [0002] Dicyclanil (dicyclanil), also known as propyrid, its chemical name is 4,6-diamino-2-cyclopropylaminopyrimidine-5-carbonitrile, is a pyrimidine compound that is an ecdysone analogue. It is a new type of insect growth regulator that is effective by interfering with the formation of insect cuticles, emphasizing the control and regulation of pest populations, and can selectively and effectively control pests. It has a high killing effect on diptera insects and fleas, and can prevent the larvae of various flies, mosquitoes and fleas from developing into pupae and adults. In addition, the drug is not easily tolerated, has low residual value, has high ecological and social benefits, and meets the requirements and goals of today's green pesticides. [0003] The domestically reported synthetic method is the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/50
CPCC07D239/50
Inventor 刘志孔庆文方明锋刘全才孔梅吴连勇
Owner QILU SYNVA PHARMA
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