Preparation method for 5-acetoacetlamino benzimdazolone

A technology of acetoacetamidobenzimidazolone and aminobenzimidazolone is applied in the field of preparation of 5-acetoacetamidobenzimidazolone, and can solve the problem of low production level and quantity of 5-acetoacetamidobenzimidazolone. The quality cannot meet the growing needs, the lack of high-performance dyes and pigments, etc., to achieve the effect of reducing the risk factor, reducing equipment requirements, and easy operation

Active Publication Date: 2014-03-26
QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP
View PDF3 Cites 19 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the dyeing pigments produced in my country cannot meet the growing needs in terms of quantity and quality, especially the high-performance dyeing pigments are scarce.
The market demand for 5-acetoacetamidobenzimidazolone is large, but the domestic production level of 5-acetoacetamidobenzimidazolone is not high enough to meet the market demand, so the production of this product has a good market prospect
In the existing process, the acetylation reaction is required to be carried out at normal pressure and at a temperature of 110-120°C. However, due to the pressure generated by the reaction itself, it is necessary to continuously release the pressure during the reaction process. Such a process operation is undoubtedly harmful to production safety. The requirements are relatively high, but there are still unavoidable safety problems in actual production

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method for 5-acetoacetlamino benzimdazolone

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0027] The invention provides a kind of preparation method of 5-acetoacetylamino benzimidazolone, comprising the following steps:

[0028] Under the action of an acid catalyst, react 5-aminobenzimidazolone, diketene, alcohol and water to obtain 5-acetoacetamidobenzimidazolone;

[0029] The alcohol is one or more of methanol, ethanol and propanol.

[0030] The preparation method provided by the present invention uses an acidic catalyst, and uses alcohol water as a solvent, which increases the solubility of 5-aminophenyl imidazolone, thereby promoting the acetylation reaction and reducing the reaction temperature, so that the reaction itself will not generate pressure. There is no need to continuously release pressure during the reaction process, thereby reducing the requirements for equipment, and also reducing the risk factor in actual production, making the reaction conditions mild and easy to operate.

[0031] All the raw materials of the present invention have no special l...

Embodiment 1

[0048] First, under the protection of nitrogen, 400 kg of o-phenylenediamine, 400 kg of urea, 3.7 kg of benzyltriethylammonium chloride, and 1000 kg of chlorobenzene were added to the reactor, and the temperature was raised to 115°C for reaction. After 8 hours of reaction, To obtain the benzimidazolone solution, slowly add 260 kg of concentrated nitric acid with a mass content of 62% to it, react at 80°C for 3 hours, then cool down to 50°C, and distill p-chlorine under reduced pressure under 0.04Mpa pressure Benzene is recovered. After the recovery is completed, 2000 kg of deionized water is added to the reactor, boiled at a temperature of 80° C. for 3 hours for purification, and finally the obtained material is dried to obtain 5-nitrobenzimidazolone.

[0049] Then 200 kilograms of 5-nitrobenzimidazolone obtained by the above steps, 60 kilograms of hydrochloric acid with a mass content of 30%, and 180 kilograms of iron powder with a mass content of 75% are mixed with 4000 kilog...

Embodiment 2

[0054] First, under the protection of nitrogen, 400 kg of o-phenylenediamine, 400 kg of urea, 3.2 kg of tetrabutylammonium bromide, and 1000 kg of chlorobenzene were added to the reactor, and the temperature was raised to 115°C for reaction. After 8 hours of reaction, benzene was obtained. and imidazolone solution, and then slowly add 255 kg of concentrated nitric acid with a mass content of 62%, react at 80°C for 3 hours, then cool down to 50°C, and distill p-chlorobenzene under reduced pressure under 0.04Mpa pressure Recovery, after the recovery is completed, add 2000 kg of deionized water to the reaction kettle, boil in water for 3 hours at a temperature of 80° C., and perform purification treatment. Finally, the obtained material is dried to obtain 5-nitrobenzimidazolone.

[0055] Then 190 kilograms of 5-nitrobenzimidazolone obtained by the above steps, 58 kilograms of hydrochloric acid with a mass content of 30%, and 175 kilograms of iron powder with a mass content of 75% ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
melting pointaaaaaaaaaa
purityaaaaaaaaaa
Login to view more

Abstract

The invention provides a preparation method for 5-acetoacetlamino benzimdazolone. The method comprises the following step of enabling 5-aminobenzimidazolone, diketene, alcohol and water to react in the presence of an acid catalyst to obtain the 5-acetoacetlamino benzimdazolone, wherein the alcohol is one or more of methanol, ethanol and propanol. According to the preparation method, the reaction temperature of an acetylation process in a production process of the 5-acetoacetlamino benzimdazolone is lowered, so that requirements on equipment are lowered, the danger coefficient during actual production is also lowered, reaction conditions are mild, and the method is easy to operate.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of 5-acetoacetamido benzimidazolone. Background technique [0002] 5-Acetoacetamidobenzimidazolone, also known as AABI, has the molecular formula C 11 h 11 N 3 o 3 , having the structure of formula I, light yellow or white crystal, is an important organic synthesis intermediate, [0003] [0004] 5-Acetoacetamidobenzimidazolone is an important chemical intermediate, which is mostly used in organic synthesis, dye intermediates, pharmaceutical intermediates, and photographic industry, especially in the field of dyeing pigments and special material synthesis, and is mostly used in the synthesis of pigments Yellow and pigment orange, etc., which are also key intermediates for the synthesis of high-performance pigments - benzimidazolone series. [0005] With the development of my country's industrial production and the improvement of ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07D235/26
CPCC07D235/26
Inventor 卢克磊陈安源陈晓涛
Owner QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap