Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for preparing intermediate diethyl acetamidomalonate through organic synthesis

A technology for producing diethyl acetamidomalonate and diethyl oximinomalonate is applied in the field of preparation of important organic synthesis intermediate diethyl acetamidomalonate, achieving low cost, high product purity, The effect of little environmental pollution

Inactive Publication Date: 2014-07-16
SUZHOU TIANMA SPECIALTY CHEM
View PDF1 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few domestic research reports on the synthetic method of the organic synthesis intermediate acetamidodiethyl malonate, so researching the preparation method of acetamidodiethylmalonate has important industrial application value

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
  • Method for preparing intermediate diethyl acetamidomalonate through organic synthesis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment one: a kind of preparation method of organic synthesis intermediate acetamidomalonate diethyl ester

[0020] In a 500 mL four-necked flask equipped with a thermometer, add 69 g of water, 80 g of diethyl malonate, 69 g of sodium nitrite, and 0.3 g of tetrabutylammonium bromide as a phase transfer catalyst. 58.3 ml of acetic acid was added dropwise, and the dropwise addition was completed in about 1 h. After the dropwise addition was completed, the reaction was carried out at 30-40 °C for 4 h. Add 50 ml of water and 300 ml of dichloromethane for extraction, combine the organic phases, add anhydrous sodium sulfate and dry overnight. The precipitate was filtered off, and the filtrate was added to a 1000ml four-neck flask.

[0021] A condenser tube was added to a 1000ml four-necked flask, and the solvent was distilled off under reduced pressure. Then add 130kg of acetic anhydride, 300ml of glacial acetic acid, and slowly add 110g of zinc powder at room temperat...

Embodiment 2

[0022] Embodiment 2: a kind of preparation method of organic synthesis intermediate acetamidomalonate diethyl ester

[0023] In the enamel reaction kettle of 1000L equipped with tail gas absorption system, add water 200kg, open stirring, add diethyl malonate 160kg, sodium nitrite 140kg, phase transfer catalyst tetrabutylammonium bromide 1kg successively, cool to 5 ℃, 120L of acetic acid was added dropwise, and the dropwise addition was completed in about 3h. After the dropwise addition, the reaction was carried out at 35~40°C for 4h. Add 60kg of water and dichloromethane to extract twice, each time 300L of dichloroethane, the organic phases are combined and dried with anhydrous sodium sulfate for 6 hours.

[0024] After drying, the filtration was completed, and the filtrate was added to a 2000L enamel reaction kettle, and the solvent was distilled off under reduced pressure. Then add 260kg of acetic anhydride, 600kg of acetic acid, and slowly add 220kg of zinc powder at norm...

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 discloses a method for preparing an intermediate diethyl acetamidomalonate through organic synthesis. The preparation method is characterized by comprising the following steps of preparing oximinodiethyl malonate by using water as a solvent, using diethyl malonate, sodium nitrite and acetic acid as raw materials and adding a phase transfer catalyst; extracting oximinodiethyl malonate by using an organic solvent, and then distilling to remove the organic solvent; adding acetic acid into the system obtained in the third step, and adding zinc powder at 40-50 DEG C to perform reduction and acetic anhydride acylation; then removing the acetic acid solvent under reduced pressure, and crystallizing with water to obtain the diethyl acetamidomalonate product, wherein the reaction temperature of the reduction and acetic anhydride acylation is 40-50 DEG C, and the reaction time is 1-6.5 hours. The yield of diethyl acetamidomalonate obtained through the preparation method reaches over 80%, the purity of the product is high, the energy consumption is low, the environmental pollution is low, and the cost is low.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of an important organic synthesis intermediate, diethyl acetamidomalonate. Background technique [0002] Diethyl acetamidomalonate is an important intermediate in organic synthesis, especially an indispensable raw material in amino acid synthesis. It is mainly used in the synthesis of rebamipide in medicine. [0003] The chemical name is: diethyl acetamidomalonate; [0004] Molecular formula: C 9 H 15 NO 5 ; [0005] Molecular weight: 217.22; [0006] The molecular formula is: [0007] [0008] Its appearance is white crystalline powder, and its melting point is 96.2~98.1℃. At present, there are few research reports disclosed domestically about the synthetic method of the organic synthesis intermediate diethyl acetamidomalonate, so research on the preparation method of diethyl acetamidomalonate has important industrial applica...

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): C07C233/47C07C231/10
Inventor 徐峰徐国良徐斌徐敏
Owner SUZHOU TIANMA SPECIALTY CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com