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Synthetic method for anti-leptospira drug ethyl imidazolate

A technology of imidazolate ethyl ester and a synthetic method, which is applied in the direction of organic chemistry, can solve the problems of high equipment corrosion resistance, increased production cost, complex process, etc., and achieve the reduction of equipment corrosion resistance and low production cost. The effect of reducing and increasing the reaction yield

Inactive Publication Date: 2018-07-03
CHENGDU QIANYE LONGHUA PETROLEUM ENG TECH CONSULTING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because this synthesis method needs to use nitric acid solution as reactant, it requires higher corrosion resistance of equipment, increased production cost, more complicated process, and the final yield is not high, generally only about 80%, so it is necessary to propose A new synthetic method

Method used

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  • Synthetic method for anti-leptospira drug ethyl imidazolate

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Experimental program
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Effect test

Embodiment 1

[0015] The synthetic method of anti-leptospirosis drug ethyl imidazole comprises the steps:

[0016] A: Add 2mol ethyl 2,5-dihydroxyimidazole-4-carboxylate and 1.9L potassium sulfate solution with a mass fraction of 15% in the reaction vessel, control the stirring speed to 210rpm, increase the temperature to 30°C, and continue the reaction for 90min ;

[0017] B: Raise the temperature to 40°C, add 6mol dicyclohexylamine solution with a mass fraction of 30%, add 3mol octacarbonyl dicobalt powder in 4 times, continue the reaction for 2h, lower the temperature to 10°C, precipitate solid, use 1.2L Wash 5 times with 10% sodium nitrate solution, 3 times with 40% cyclohexane solution, recrystallize in 80% tripropylene glycol monomethyl ether solution, dehydrating agent anhydrous magnesium sulfate After dehydration, 240.8 g of the finished imidazole ethyl ester was obtained, with a yield of 86%.

Embodiment 2

[0019] The synthetic method of anti-leptospirosis drug ethyl imidazole comprises the steps:

[0020] A: Add 2mol ethyl 2,5-dihydroxyimidazole-4-carboxylate and 1.9L potassium sulfate solution with a mass fraction of 18% in the reaction vessel, control the stirring speed at 230rpm, raise the temperature to 33°C, and continue the reaction for 110min ;

[0021] B: Raise the temperature to 42.5°C, add 7mol mass fraction of 33% dicyclohexylamine solution, add 3.5mol octacarbonyl dicobalt powder in 5 times, continue the reaction for 2.5.h, lower the temperature to 12.5°C, and precipitate a solid, Wash 6 times with 1.2L of 13.5% sodium nitrate solution, 4 times with 42.5% cyclohexane solution, recrystallize in 83% tripropylene glycol monomethyl ether solution, dehydrating agent activity Alumina was dehydrated to obtain 254.8 g of imidazole ethyl ester with a yield of 91%.

Embodiment 3

[0023] The synthetic method of anti-leptospirosis drug ethyl imidazole comprises the steps:

[0024] A: Add 2mol ethyl 2,5-dihydroxyimidazole-4-carboxylate and 1.9L potassium sulfate solution with a mass fraction of 21% in the reaction vessel, control the stirring speed at 250rpm, raise the temperature to 36°C, and continue the reaction for 130min ;

[0025] B: Raise the temperature to 45°C, add 8 mol of dicyclohexylamine solution with a mass fraction of 36%, add 4 mol of dicobalt octacarbonyl powder in 6 times, continue the reaction for 3 hours, lower the temperature to 15°C, precipitate a solid, and use 1.2L Wash 7 times with 17% sodium nitrate solution, 5 times with 45% cyclohexane solution, recrystallize in 86% tripropylene glycol monomethyl ether solution, dehydrating agent anhydrous magnesium sulfate After dehydration, 263.2 g of the finished imidazole ethyl ester was obtained, with a yield of 94%.

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Abstract

The invention discloses a synthetic method for the anti-leptospira drug ethyl imidazolate. The synthetic method comprises the following steps: adding ethyl 2,5-dihydroxyimidazole-4-carboxylate and a potassium sulfate solution into a reaction vessel, controlling a stirring speed, increasing a temperature, and continuing a reaction; and raising the temperature, adding a dicyclohexylamine solution, adding dicobalt octacarbonyl powder in batches, continuing the reaction, lowering the temperature, allowing a solid to be precipitated, washing the solid with a sodium nitrate solution a plurality of times, then washing the solid with a cyclohexane solution, carrying out recrystallization in a tripropylene glycol monomethyl ether solution, and then carrying out dehydration with a dehydrating agentso as to obtain the finished ethyl imidazolate.

Description

technical field [0001] The invention relates to a preparation method of medicine, which belongs to the field of organic synthesis, in particular to a synthesis method of ethyl imidazolate, an anti-leptospira drug. Background technique [0002] Ethyl imidazolate has a significant anti-leptospirosis effect. It is rapidly absorbed after oral administration, widely distributed in the body, and can enter the central nervous system through the blood-brain barrier. Most of the existing synthetic methods use ethyl 2-mercaptoimidazole-4-carboxylate and nitric acid solution as the main reactants to generate ethyl imidazolate. Because this synthesis method needs to use nitric acid solution as reactant, it requires higher corrosion resistance of equipment, increased production cost, more complicated process, and the final yield is not high, generally only about 80%, so it is necessary to propose A new synthetic method. Contents of the invention [0003] Based on the technical probl...

Claims

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Application Information

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IPC IPC(8): C07D233/90
CPCC07D233/90
Inventor 关艮安
Owner CHENGDU QIANYE LONGHUA PETROLEUM ENG TECH CONSULTING
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