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

Continuous synthesis method of diethyl methylmalonate

A technology of diethyl methylmalonate and cyanopropionic acid is applied in the field of continuous synthesis of diethyl methylmalonate, which can solve the problem of high raw material price, difficulty in obtaining, and the price of diethyl methylmalonate. Expensive and other problems, to achieve the effect of high esterification yield and simple reaction process

Inactive Publication Date: 2018-12-18
营创三征(营口)精细化工有限公司
View PDF6 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the synthesis process, the price of raw materials is relatively high and difficult to obtain, resulting in the high price of diethyl methylmalonate

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] A method for continuously synthesizing diethyl methylmalonate, the steps are as follows:

[0013] Add 2-cyanopropionic acid to ethanol to dissolve, control the molar ratio of 2-cyanopropionic acid to ethanol to be 1:4, transfer to the reaction kettle after dissolving. Stirring, under room temperature conditions, slowly add 98% concentrated sulfuric acid to the reactor from the dropping funnel, control the mass ratio of 2-cyanopropionic acid to sulfuric acid to 1:1.3, control the temperature at 60°C, and raise the system after the addition is completed The temperature is controlled at 80°C, and the reaction ends after 4 hours of reaction; at 85°C, the ethanol component in the reaction system is distilled off, and 12% ammonia water is added dropwise to the system for neutralization, the temperature is controlled at 85°C, and the pH of the feed solution is adjusted to 7- 8. Separate the crude diethyl methylmalonate in the organic phase. The diethyl methylmalonate crude p...

Embodiment 2

[0015] A method for continuously synthesizing diethyl methylmalonate, the steps are as follows:

[0016] Add 2-cyanopropionic acid to ethanol to dissolve, control the molar ratio of 2-cyanopropionic acid to ethanol to be 1:6, transfer it to the reaction kettle after dissolving; Slowly add 98wt.% concentrated sulfuric acid to the mixture, control the mass ratio of 2-cyanopropionic acid to sulfuric acid to 1:2.8, control the temperature at 65°C, increase the temperature of the system after the dropwise addition and control it at 95°C, and the reaction ends after 5 hours of reaction; At 60°C, distill out the ethanol component in the reaction system, add dropwise 12wt.% ammonia water to the reaction system for neutralization, control the temperature at 90°C, adjust the pH of the feed solution to 7, and separate diethyl methylmalonate Crude product: drop the diethyl methylmalonate crude product into rectification under reduced pressure in the rectifying tower, obtain diethyl methyl...

Embodiment 3

[0018] A method for continuously synthesizing diethyl methylmalonate, the steps are as follows:

[0019] Add 2-cyanopropionic acid to ethanol to dissolve, control the molar ratio of 2-cyanopropionic acid to ethanol to be 1:2.5, transfer it to the reaction kettle after dissolving; Slowly add 98wt.% concentrated sulfuric acid to the mixture, control the mass ratio of 2-cyanopropionic acid to sulfuric acid to 1:0.5, control the temperature at 55°C, increase the temperature of the system after the dropwise addition and control it at 70°C, and the reaction ends after 2 hours of reaction; At 45°C, distill out the ethanol component in the reaction system, add 12wt.% ammonia water dropwise to the reaction system for neutralization, control the temperature at 70°C, adjust the pH of the feed solution to 8, and separate diethyl methylmalonate Crude product: drop the diethyl methylmalonate crude product into rectification under reduced pressure in the rectifying tower, obtain diethyl meth...

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 belongs to the technical field of organic synthesis, and specifically relates to a continuous synthesis method of diethyl methylmalonate. 2-chloropropionic acid is continuously cyanidedto obtain 2-cyanopropionic acid; 2-cyanopropionic acid and ethanol carry out esterification reactions under the action of sulfuric acid to obtain a crude product of diethyl methylmalonate directly inone step; and the finished product is obtained after steps of washing and distillation. The reaction process is simple, and the yields of hydrolysis and esterification are high.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for continuously synthesizing diethyl methylmalonate. Background technique [0002] Diethyl methylmalonate is an important intermediate in organic synthesis and is widely used in the production of medicines, dyes, spices, pesticides and herbicides. In medicine, diethyl methylmalonate is mainly used in the production of muscone. At present, the synthesis of diethyl methylmalonate mainly includes heating diethyl oxalylpropionate to violently release carbon monoxide at a temperature of 130-150°C. After the released gas is reduced, gradually increase the temperature to make the liquid reflux until the gas escapes. Diethyl methylmalonate was obtained by distillation with a yield of 97%. [0003] In the synthesis process, the price of raw materials is higher and difficult to obtain, resulting in the high price of diethyl methylmalonate. Contents of the invention...

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): C07C67/08C07C67/48C07C69/38
CPCC07C67/08C07C67/48C07C69/38
Inventor 刘至寻梁海赵志刚
Owner 营创三征(营口)精细化工有限公司
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