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Method for preparing benzimidazolone in water solvent

A technology of benzimidazolone and water solvent, which is applied in the field of biological polypeptide condensing agent by-product treatment, can solve the problems of low yield, poor safety, high production cost, etc., and achieve the effect of low price, easy acquisition, and material cost saving

Inactive Publication Date: 2020-07-03
SHANDONG HUIHAI PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The purpose of the present invention is to provide a method for preparing benzimidazolone in a water solvent by overcoming the problems of poor safety, low yield and high production cost commonly existing in the prior art

Method used

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  • Method for preparing benzimidazolone in water solvent

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Effect test

Embodiment 1

[0023] Add the aqueous solution of the auxiliary agent into the reaction bottle, the auxiliary agent is sodium salt, the mass ratio of the auxiliary agent to water in the aqueous auxiliary agent solution is 1:8, start stirring, and add o-phenylenediamine and urea when the temperature rises to 130 °C, urea and o-phenylenediamine The mass ratio of phenylenediamine is 1:1.1, the mass ratio of o-phenylenediamine to the water initially added to the aqueous solution of the auxiliary agent in the reaction bottle is 2:5, and the reaction is carried out at 130°C for 5 hours. After the reaction is completed, the aqueous solution of the auxiliary agent is added for 14 , filtered with suction and rinsed with water, the filter cake was dried to obtain benzimidazolone, and the filtrate, namely the mother liquor, was concentrated and used mechanically. The yield of benzimidazolone was 99.04%, and the purity was 99.32%.

Embodiment 2

[0025] Add the aqueous solution of the auxiliary agent into the reaction bottle, the auxiliary agent is magnesium salt, the mass ratio of the auxiliary agent to water in the aqueous auxiliary agent solution is 2:15, start stirring, and add o-phenylenediamine and urea when the temperature rises to 105°C, urea and o-phenylenediamine The mass ratio of phenylenediamine is 1:1, the mass ratio of o-phenylenediamine to the water initially added to the aqueous solution of the auxiliary agent in the reaction bottle is 1:3, and the reaction is carried out at 105°C for 3 hours. After the reaction is completed, the aqueous solution of the auxiliary agent is added. Suction filtration and rinse with water, the filter cake is dried to benzimidazolone, the filtrate, namely the mother liquor, is concentrated and used mechanically, the yield of benzimidazolone is 99.19%, and the purity is 99.61%.

Embodiment 3

[0027] Add the aqueous solution of the auxiliary agent into the reaction bottle, the auxiliary agent is a mixture of aluminum salt and zinc salt, the mass ratio of the auxiliary agent to water in the aqueous auxiliary agent solution is 1.1:20, start stirring, and add o-phenylenediamine and Urea, the mass ratio of urea to o-phenylenediamine is 1:1.2, the mass ratio of o-phenylenediamine to the water initially added to the auxiliary agent aqueous solution in the reaction bottle is 1:4, and the reaction is carried out at 90°C for 7 hours. After the reaction is completed, Aqueous additive solution is added, suction filtered and rinsed with water, the filter cake is dried to obtain benzimidazolone, and the filtrate, mother liquor, is concentrated and used mechanically. The yield of benzimidazolone is 99.53%, and the purity is 99.78%.

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Abstract

The invention discloses a method for preparing benzimidazolone in a water solvent. The method comprises the following steps: adding an aqueous solution of an additive into a reaction bottle, startingstirring, carrying out heating to 90-140 DEG C, adding o-phenylenediamine and urea, carrying out a heat-preserved reaction for 3-8 h, adding the aqueous solution of the additive or mother liquor afterthe reaction is completed, carrying out suction filtration, performing leaching with water to obtain a solid material which is benzimidazolone, indiscriminately using the mother liquor, concentratinga leaching solution, and indiscriminately using the leaching solution. A technical scheme for synthesizing benzimidazolone by taking water as a solvent under the condition of normal pressure is realized, the yield of benzimidazolone is greater than 99%, and the purity of benzimidazolone is greater than 99%. The method of the invention uses water as a solvent and realizes indiscriminate usage of the mother liquor, so the method is environment-friendly, safe and feasible, and is low in production cost and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of biological polypeptide condensing agent by-product treatment, and in particular relates to a method for preparing benzimidazolone in a water solvent. Background technique [0002] Benzimidazolone is an important organic intermediate, especially used in the fields of medicine, pigment and pesticide. [0003] J.Am.Chem.Soc.80,1657 (1958) discloses a method for preparing benzimidazolone by reacting o-phenylenediamine and phosgene. However, the phosgene used in this method is highly dangerous, and the by-product hydrogen chloride generated by the reaction is highly corrosive to equipment. [0004] In US-4138568, o-phenylenediamine compounds react with urea and urea derivatives in a water-insoluble organic solvent at a temperature of 100°C to 200°C to obtain benzimidazolone, and then undergo a complicated purification process, solvent consumption Large, producing a large amount of waste liquid. [0005] In DE2052026,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D235/26
CPCC07D235/26
Inventor 张国辉姜福元张翠翠付德修王磊侯绪会王亮亮
Owner SHANDONG HUIHAI PHARMA & CHEM
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