Supercharge Your Innovation With Domain-Expert AI Agents!

Method of preparing malonate diester by using malic acid as raw material

A technology of malonate diester and malic acid, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of no synthesis of malonate diester, etc., and achieve an efficient reaction process Effect

Active Publication Date: 2014-09-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
View PDF9 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there is no research report on the synthesis of malonate diester from malic acid in the literature

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 of preparing malonate diester by using malic acid as raw material
  • Method of preparing malonate diester by using malic acid as raw material
  • Method of preparing malonate diester by using malic acid as raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: With 0.3350g malic acid, 1mol% (relative to raw material malic acid) phosphomolybdovanadium heteropolyacid, join in the 35mL reactor, add 3mL methanol, close the kettle, fill in the oxygen pressure and be 1.0MPa, under stirring Raise the temperature to 90°C and keep it for 6h. It was then cooled to room temperature and carefully depressurized to atmospheric pressure. All the products were transferred to the volumetric flask, after adding the internal standard naphthalene, the volume was constant with acetonitrile, and then the samples were analyzed by gas chromatography (GC, figure 1 ), internal standard quantitative method obtains the selectivity of malonate diester in the product. According to the calculation of formula malonate diester selectivity=(mass amount of malonate diester) / (sum of the amount of all product substances after the reaction), the selectivity of malonate diester is 59.6%. Use GC-MS and gas chromatographic retention time of standard ...

Embodiment 2

[0017] Embodiment 2: With 0.3350g malic acid, 1mol% (relative to raw material malic acid) vanadyl sulfate, join in the 35mL reactor, add 3mL methanol, close the kettle, fill in oxygen pressure and be 1.0MPa, be heated up to 100 under stirring ℃, and keep for 6h. It was then cooled to room temperature and carefully depressurized to atmospheric pressure. The product was analyzed according to the method in Example 1, and the selectivity of malonate diester was 76.1%.

Embodiment 3

[0018] Embodiment 3: With 0.3350g malic acid, 1mol% (relative to raw material malic acid) vanadyl acetylacetonate, join in the 35mL reactor, add 3mL methanol, close the kettle, fill in oxygen pressure and be 1.0MPa, be heated up to under stirring 100°C and keep for 4h. It was then cooled to room temperature and carefully depressurized to atmospheric pressure. The product was analyzed according to the method in Example 1, and the selectivity of malonate diester was 70.5%.

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 new method of preparing malonate diester by using malic acid as a raw material. According to the method, oxygen or air is used as an oxygen source, alcohol is used as a solvent, vanadium oxide is used as a catalyst, and the malic acid is converted into the malonate diester by one step through coupling an esterification reaction and an oxidation reaction. The raw material malic acid can be obtained from biomass resources, halogen, cyanide and other toxic substances are not used during a whole process, and thus the method is wide in application prospect.

Description

technical field [0001] The present invention reports a new method for preparing malonate diester with malic acid as raw material, specifically using air or oxygen as oxygen source, alcohol as solvent, vanadium oxy compound as catalyst, through oxidation reaction and esterification reaction The coupling directly converts malate to malonate diester. Background technique [0002] The hydrogen atom on the active methylene group in the malonate diester molecule is easy to react with other groups, so it can undergo various reactions such as alkylation, hydroxyalkylation, and amidation. An important intermediate of various fine chemicals such as spices. [0003] The traditional preparation route of malonate diester mainly adopts the sodium cyanide method, which uses chloroacetic acid, sodium cyanide and alcohol as raw materials, and undergoes neutralization, cyanation, acidification, esterification, etc. For example, in industry, the production process of diethyl malonate is, fir...

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 Patents(China)
IPC IPC(8): C07C69/38C07C67/08
Inventor 徐杰刘俊霞杜中田杨艳良高进苗虹
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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