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Preparation method of high-purity 5-acetylacetylaminobenzimidazolone

A technology of acetoacetamidobenzimidazolone and aminobenzimidazolone, which is applied in the field of preparation of high-purity 5-acetoacetamidobenzimidazolone, and can solve the problems of large environmental pollution, high production cost, poor safety, etc. problems, to achieve the effects of reducing environmental hazards, low production costs, and small environmental impacts

Inactive Publication Date: 2019-01-18
SHANDONG HUIHAI PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a preparation method of high-purity 5-acetoacetamido benzimidazolone, which overcomes the common problems of poor safety, large environmental pollution and high production cost in the prior art.

Method used

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  • Preparation method of high-purity 5-acetylacetylaminobenzimidazolone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add water 3700kg in reactor, wet weight is 51% 5-acetamidobenzimidazolone 285kg, sodium bisulfite 16kg, mass fraction is 20kg of hydrochloric acid of 30%, activated carbon 20kg starts to stir, is warming up to 68 ℃, reacts Press filter for 1 hour, heat up the filtrate to 60° C., add 20 kg of sodium hydroxide and 108 kg of diketene to react for 4 hours, cool down and press filter to obtain 5-acetoacetamido benzimidazolone.

[0026] The 5-acetoacetamidobenzimidazolone obtained by the above examples of the present invention is detected by liquid chromatography, the purity of the 5-acetoacetamidobenzimidazolone prepared by the present invention is 99.5013%, the raw material peak is 0.0152%, and the acetic anhydride peak is 0.1506%, in line with industry standards.

[0027] The 5-acetoacetamidobenzimidazolone obtained in the above example of the present invention is detected, and the yield of the 5-acetoacetamidobenzimidazolone prepared in the present invention is 88.13%.

Embodiment 2

[0029] Add water 3700kg in the reactor, wet weight is 50% 5-acetamidobenzimidazolone 285kg, sodium bisulfite 16kg, mass fraction is 30% sulfuric acid 10kg, gac 20kg starts to stir, is warming up to 65 ℃, reacts Press filter for 1 hour, heat up the filtrate to 60° C., add 20 kg of sodium hydroxide and 108 kg of diketene to react for 4 hours, cool down and press filter to obtain 5-acetoacetamido benzimidazolone.

[0030] The 5-acetoacetamidobenzimidazolone obtained by the above examples of the present invention is detected by liquid chromatography, the purity of the 5-acetoacetamidobenzimidazolone prepared by the present invention is 99.6196%, the raw material peak is 0.0110%, and the acetic anhydride peak is 0.1769%, in line with industry standards.

[0031] The 5-acetoacetamidobenzimidazolone obtained in the above example of the present invention was detected, and the yield of the 5-acetoacetamidobenzimidazolone prepared in the present invention was 86.52%.

Embodiment 3

[0033] Add 3700kg of water in the reactor, 280kg of 5-acetamidobenzimidazolone with a wet weight of 48%, 15kg of sodium bisulfite, 22kg of hydrochloric acid with a mass fraction of 30%, and 20kg of activated carbon to start stirring, heat up to 66°C, and react Press filter for 1 hour, heat up the filtrate to 60° C., add 22 kg of sodium hydroxide and 108 kg of diketene to react for 4 hours, cool down and press filter to obtain 5-acetoacetamido benzimidazolone.

[0034] The 5-acetoacetamidobenzimidazolone obtained by the above examples of the present invention is detected by liquid chromatography, the purity of the 5-acetoacetamidobenzimidazolone prepared by the present invention is 99.6351%, the raw material peak is 0.0156%, and the acetic anhydride peak is 0.0888%, in line with industry standards.

[0035] The 5-acetoacetamidobenzimidazolone obtained in the above example of the present invention is detected, and the yield of the 5-acetoacetamidobenzimidazolone prepared in the ...

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Abstract

The invention discloses a preparation method of high-purity 5-acetylacetylaminobenzimidazolone. According to the technical essentials, the preparation method comprises the following steps: under an acidic condition, adding 5-aminobenzimidazolone, sodium hydrogen sulfite, activated carbon and water and reacting at 65 to 70 DEG C; performing suction filtration to obtain intermediate filtrate; addingdiketene and sodium hydroxide into the filtrate and reacting at 60 to 65 DEG C to obtain the 5-acetylacetylaminobenzimidazolone. The purity of a product obtained by the preparation method is greaterthan 99.5 percent and the yield is greater than 87 percent. The preparation method disclosed by the invention has the advantages of simple and easy-to-control technology, safety in operation, small influences on environment and low production cost.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and more specifically relates to a method for preparing high-purity 5-acetoacetamido benzimidazolone. Background technique [0002] 5-Acetoacetylaminobenzimidazolone is a white or off-white crystal, which is mostly used in the synthesis of high-performance dyes-imidazolone series. [0003] 5-Acetoacetylaminobenzimidazolone, English name: 5-acetylacetamidobenzimidazolone, referred to as AABI, molecular formula is C 11 h 11 N 3 o 3 , with a relative molecular mass of 233.22, is an important chemical raw material intermediate, mostly used in the synthesis of dye orange and dye yellow. At present, the method for large-scale production of 5-acetoacetamidobenzimidazolone both at home and abroad is to react 5-aminobenzimidazolone with diketene, alcohol and water under acidic conditions to obtain 5-acetoacetamidobenzimidazolone. But its disadvantages are obvious, mainly: 1. The solvent use...

Claims

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Application Information

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IPC IPC(8): C07D235/26
CPCC07D235/26
Inventor 付德修李宁张国辉王磊李华振侯绪会张翠翠
Owner SHANDONG HUIHAI PHARMA & CHEM
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