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Method for improving quality of 5-acetoacetlaminobenzimdazolone

A technology of acetoacetamidobenzimidazolone and aminobenzimidazolone, which is applied in the field of chemical synthesis, can solve problems such as the use of downstream customers that affect product quality, and achieve the effects of reducing environmental protection investment, improving utilization rate and reducing waste amount

Inactive Publication Date: 2019-08-16
SHANDONG HUIHAI PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method of large-scale production of 5-acetoacetamidobenzimidazolone at home and abroad is to react 5-aminobenzimidazolone and diketene under acidic conditions to obtain 5-acetoacetamidobenzimidazolone, but its disadvantages Obviously, the main reason is: diketene contains acetic anhydride, the content of acetic anhydride is about 1.4%, and the peak of acetic anhydride is easy to form during the reaction process, and the content is about 0.55%, which seriously affects the quality of the product and the use of downstream customers

Method used

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  • Method for improving quality of 5-acetoacetlaminobenzimdazolone

Examples

Experimental program
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Effect test

Embodiment 1

[0024] A method for improving the quality of 5-acetoacetamido benzimidazolone, comprising the following steps:

[0025] 1) Diketene and water are pretreated at -10°C in a mass ratio of 1:66 to obtain a diketene solution;

[0026] 2) Add water and 5-aminobenzimidazolone with a wet weight of 51% into the reaction kettle, the mass ratio of 5-aminobenzimidazolone to water is 13:40, heat up to 75°C, keep it warm for 30 minutes, turn to Feed to the acylation tank;

[0027] 3) Add the pretreated diketene solution dropwise into the acylation kettle, the mass ratio of diketene to 5-aminobenzimidazolone is 1:3, keep it warm for 30 minutes, cool down to 45°C, press the material, and dry to obtain 5- Acetoacetamidobenzimidazolone. The content of 5-acetoacetylaminobenzimidazolone is 99.61%, and the content of by-product 5-acetylaminobenzimidazolone is 0.19%.

[0028] In step 2), sodium bisulfite and activated carbon are also added into the reaction kettle, and the mass ratio of sodium b...

Embodiment 2

[0031] A method for improving the quality of 5-acetoacetamido benzimidazolone, comprising the following steps:

[0032] 1) Diketene and water are pretreated at 0°C in a mass ratio of 1:65 to obtain a diketene solution;

[0033] 2) Add water and 5-aminobenzimidazolone with a wet weight of 51% into the reaction kettle, the mass ratio of 5-aminobenzimidazolone to water is 11:30, heat up to 80°C, keep it warm for 30 minutes, turn to Feed to the acylation tank;

[0034] 3) Add the pretreated diketene solution dropwise into the acylation kettle, the mass ratio of diketene to 5-aminobenzimidazolone is 1:2.5, keep it warm for 35 minutes, cool down to 45°C, press the material, and dry to obtain 5- Acetoacetamidobenzimidazolone. The content of 5-acetoacetylaminobenzimidazolone is 99.64%, and the content of by-product 5-acetylaminobenzimidazolone is 0.16%.

[0035] In step 2), sodium bisulfite and activated carbon are also added to the reactor, and the mass ratio of sodium bisulfite, ...

Embodiment 3

[0038] A method for improving the quality of 5-acetoacetamido benzimidazolone, comprising the following steps:

[0039] 1) Diketene and water are pretreated at -5°C in a mass ratio of 1:62 to obtain a diketene solution;

[0040] 2) Add water and 5-aminobenzimidazolone with a wet weight of 51% into the reaction kettle, the mass ratio of 5-aminobenzimidazolone to water is 12:35, heat up to 85°C, keep it warm for 25 minutes, turn to Feed to the acylation tank;

[0041] 3) Add the pretreated diketene solution dropwise into the acylation kettle, the mass ratio of diketene to 5-aminobenzimidazolone is 1:2, keep it warm for 40 minutes, cool down to 40°C, press the material, and dry to obtain 5- Acetoacetamidobenzimidazolone. The content of 5-acetoacetylaminobenzimidazolone is 99.60%, and the content of by-product 5-acetylaminobenzimidazolone is 0.20%.

[0042] In step 2), sodium bisulfite and activated carbon are also added to the reactor, and the mass ratio of sodium bisulfite, a...

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Abstract

The invention relates to a method for improving the quality of 5-acetoacetlaminobenzimdazolone. The method comprises the following steps: pre-treating diketene and water at a low temperature to make acetic anhydride in diketene react with water to form acetic acid, then raising the temperature and dropwise adding the treated diketene into 5-aminobenzimidazolone, performing heat preservation for 30min, performing cooling to 45 DEG C, performing material pressing, and performing drying to obtain 5-acetoacetlaminobenzimdazolone. After the pretreatment of diketene and water at the low temperature, acetic anhydride in diketene can be reacted with water to form acetic acid, the purity of diketene is improved, and thus the product purity is improved, the product yield is improved, and the content of 5-acetoacetlaminobenzimdazolone after the treatment is up to 99.6%. The formation of the by-product 5-acetylaminobenzimidazolone is reduced, the by-product content is decreased to be 0.2%, the final product yield is increased, the utilization rate of raw materials is improved, the waste material amount is reduced, the environmental protection investment is reduced, and the production cost isreduced.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for improving the quality of 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. 5-Acetoacetylaminobenzimidazolone, English name: 5-acetylacetamidobenzimidazolone, referred to as AABI, molecular formula is C 11 h 11 N 3 O3, with a relative molecular mass of 233.22, is an important intermediate of chemical raw materials, and is mostly used in the synthesis of dye orange and dye yellow. At present, the method of large-scale production of 5-acetoacetamidobenzimidazolone at home and abroad is to react 5-aminobenzimidazolone and diketene under acidic conditions to obtain 5-acetoacetamidobenzimidazolone, but its disadvantages Obviously, the main reason is that diketene contains acetic anhydr...

Claims

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Application Information

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IPC IPC(8): C07D235/26
CPCC07D235/26
Inventor 赵攀峰殷福东苏倩王亮亮张国辉张忠政
Owner SHANDONG HUIHAI PHARMA & CHEM
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