Check patentability & draft patents in minutes with Patsnap Eureka AI!

Synthesis method of high-purity N-ethoxycarbonyl-2, 3-disubstituted maleimide

A technology of dimethyl butenedimide and butenedimide is applied in the field of N-ethoxycarbonyl-2 and can solve the problem of N-ethoxycarbonyl-2,3-disubstituted butenedioyl The purity of imine is not high enough, and it cannot meet the development requirements of enzyme-specific kits, so as to achieve the effect of simple operation, good market application value and convenient operation.

Active Publication Date: 2018-10-09
ANQING NORMAL UNIV
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far, the purity of N-ethoxycarbonyl-2,3-disubstituted butenedimides obtained by existing methods is not high enough to meet the development requirements of the above-mentioned enzyme-specific kits

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
  • Synthesis method of high-purity N-ethoxycarbonyl-2, 3-disubstituted maleimide
  • Synthesis method of high-purity N-ethoxycarbonyl-2, 3-disubstituted maleimide
  • Synthesis method of high-purity N-ethoxycarbonyl-2, 3-disubstituted maleimide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The synthetic method of a kind of high-purity N-ethoxycarbonyl-2,3-disubstituted butenedimide of the present embodiment comprises the following steps:

[0023] (1) Preparation of 2,3-dimethylbutenediimide

[0024] A. Dissolve 1.0g of 3,4-dimethylfuran-2,5-dione (structural formula shown in formula 1) in 10mL of DMF, add 17mL of hexamethyldisilazane HMDS and 1.7mL of Methanol was added and reacted at room temperature for 1 h, and then the corresponding solvent was evaporated to dryness using a rotary evaporator;

[0025]

[0026] B. Add 4mL DMF, 17mL HMDS and 1.7mL methanol to react for 7 hours, then add 65mL water and 45mL ethyl acetate for extraction, and extract twice;

[0027] C. Merge the organic phases, and wash the extract with water and saturated brine, then dry it with anhydrous sodium sulfate drying method, evaporate the solvent, and dry it with an oil pump to obtain 0.9 g of white solid, namely 2,3-dimethyl Butene imide (structural formula shown in formul...

Embodiment 2

[0034] The synthetic method of a kind of high-purity N-ethoxycarbonyl-2,3-disubstituted butenedimide of the present embodiment comprises the following steps:

[0035] (1) Preparation of 2,3-dimethylbutenediimide

[0036] A. Dissolve 1.2g of 3,4-dimethylfuran-2,5-dione (structural formula shown in Formula 1) in 12mL of DMF, add 19mL of hexamethyldisilazane HMDS and 1.9mL of Methanol was added and reacted at room temperature for 3 hours, and then the corresponding solvent was evaporated to dryness using a rotary evaporator;

[0037]

[0038] B. Add 6 mL of DMF, 19 mL of HMDS and 1.9 mL of methanol to react for 9 hours, then add 75 mL of water and 55 mL of ethyl acetate for extraction, and extract 4 times;

[0039] C. Merge the organic phases, and wash the extract with water and saturated brine, then dry it with anhydrous sodium sulfate drying method, evaporate the solvent, and dry it with an oil pump to obtain 1.1 g of white solid, namely 2,3-dimethyl Butene imide (structur...

Embodiment 3

[0046] The synthetic method of a kind of high-purity N-ethoxycarbonyl-2,3-disubstituted butenedimide of the present embodiment comprises the following steps:

[0047] (1) Preparation of 2,3-dimethylbutenediimide

[0048] A. Dissolve 1.1g of 3,4-dimethylfuran-2,5-dione (structural formula shown in formula 1) in 11mL of DMF, add 18mL of hexamethyldisilazane HMDS and 1.8mL of Methanol was added and reacted at room temperature for 2 hours, and then the corresponding solvent was evaporated to dryness using a rotary evaporator;

[0049]

[0050] B. Add 5mL DMF, 18mL HMDS and 1.8mL methanol to react for 8 hours, then add 70mL water and 50mL ethyl acetate for extraction, and extract 3 times;

[0051] C. Merge the organic phases, and wash the extract with water and saturated brine, then dry it with anhydrous sodium sulfate drying method, evaporate the solvent, and dry it with an oil pump to obtain 1.0 g of white solid, namely 2,3-dimethyl Butylene imide (structural formula shown in ...

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

No PUM Login to View More

Abstract

The invention provides a synthesis method of high-purity N-ethoxycarbonyl-2, 3-disubstituted maleimide. The method comprises (1) dissolving 3, 4-dimethylfuran-2, 5-dione in DMF, adding HMDS and methanol into the solution under an ice bath for a reaction at the room temperature, carrying out rotary evaporation to remove a solvent, adding DMF, HMDS and methanol into the product for a reaction, carrying out extraction, mixing the organic phases, carrying out washing through water and a saturated table salt solution, carrying out drying, carrying out evaporation to remove the solvent and drying the solution through an oil pump to obtain 2, 3-dimethylbutenedimide, and (2) gradually adding ethyl chloroformate into an ethyl acetate mixed solution of 2, 3-dimethylmaleimide and N-methylmorpholine,carrying out a reaction process at the room temperature, carrying out washing with water, saturated table salt water and dilute hydrochloric acid and carrying out drying and evaporation to obtain a desired product. The synthesis method can efficiently acquire N-ethoxycarbonyl-2, 3-disubstituted maleimide with high purity for biological kit development, and has a good market application value.

Description

technical field [0001] The present invention relates to the field of preparation of N-ethoxycarbonyl-2,3-disubstituted butenediimide, in particular to a high-purity N-ethoxycarbonyl-2,3-disubstituted butenedimide synthetic method. Background technique [0002] N-ethoxycarbonyl-2,3-disubstituted butenediimide is a special kind of organic synthesis cutting block necessary for the construction of enzyme-specific kits. It is used to modify DNA polymerase and keep its enzyme activity thermally stable. properties, so that it has the ability to be made into a kit; for the entire enzyme kit, the purity of N-ethoxycarbonyl-2,3-disubstituted butenedimide will directly affect the final detection of the enzyme kit result. Accordingly, the synthesis and development of high-purity N-ethoxycarbonyl-2,3-disubstituted butenedimide will have extremely important practical significance. However, so far, the purity of N-ethoxycarbonyl-2,3-disubstituted butenedimide obtained by the existing me...

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): C07D207/452
CPCC07D207/452
Inventor 陈太杰冯依玲徐衡王志远严达黄荣谊
Owner ANQING NORMAL UNIV
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com