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

Method for preparing dicyclohexylcarbodiimide by using vilsmeier reagent

A technology of dicyclohexylcarbodiimide and dicyclohexylurea, which is applied in the field of preparing dicyclohexylcarbodiimide, can solve problems such as insufficiently stable yield, insufficiently high yield, and adverse effects of industrial production, and achieve operational The effect of simplicity and mild process conditions

Inactive Publication Date: 2020-12-15
SHANDONG JINCHENG KERUI CHEMICAL CO LTD
View PDF3 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of relatively safe solid phosgene in this process can effectively ensure safety and environmental protection, and fundamentally eliminate the problem of serious pollution of the three wastes, but the yield of this process is not stable enough and the yield is not high enough, which will adversely affect future industrial 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
  • Method for preparing dicyclohexylcarbodiimide by using vilsmeier reagent
  • Method for preparing dicyclohexylcarbodiimide by using vilsmeier reagent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 3g DMF to 40g SOCl 2 , stirred for 30min and set aside. Put 50g of DCU and 400mL of dichloromethane into a dry 500mL three-neck flask, and stir evenly. will prepare SOCl 2 / DMF solution was added dropwise to the there-necked flask, the time for the controlled addition was 2h, and the temperature for the addition was 10°C. After the addition, the stirring reaction was continued for 5h. After the reaction, the reaction solution was added dropwise to 410g of a 10% NaOH aqueous solution. Then suction filtration, the filtrate was distilled under normal pressure to remove the solvent, and then distilled under reduced pressure at a pressure of 1.35-1.54KPa to collect fractions at 153-156°C and vacuum-dried to obtain the product with a purity of 95.8% and a yield of 87.5%.

[0023] Carry out nuclear magnetic test to above-mentioned product, record proton nuclear magnetic spectrum spectrogram such as figure 1 shown.

Embodiment 2

[0025] Add 4.5g DMF to 52g SOCl 2 , stirred for 30min and set aside. Put 50g of DCU and 300mL of dichloromethane into a dry 500mL three-neck flask, and stir evenly. will prepare SOCl 2 / DMF solution is added dropwise to the three-necked flask, the dropping time is controlled to be 0.5h, the dropping temperature is 30°C, and the stirring reaction is continued for 5h after the dropping is completed. , and then suction filtered, the filtrate was distilled under normal pressure to remove the solvent, then distilled under reduced pressure at 1.35-1.54KPa to collect fractions at 153-156°C, and vacuum dried to obtain the product with a purity of 98.9% and a yield of 92.4%.

Embodiment 3

[0027] Add 3g DMF to 48g SOCl 2 , stirred for 30min and set aside. Put 50g of DCU and 500mL of dichloromethane into a dry 500mL three-neck flask, and stir evenly. will prepare SOCl 2 / DMF solution is added dropwise to the three-necked flask, the dropping time is controlled to be 0.5h, the dropping temperature is 30°C, and the stirring reaction is continued for 2h after the dropping is completed. , and then suction filtered, the filtrate was distilled under normal pressure to remove the solvent, then distilled under reduced pressure at 1.35-1.54KPa to collect fractions at 153-156°C, and vacuum dried to obtain the product with a purity of 96.7% and a yield of 90.9%.

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 dicyclohexylcarbodiimide by using a vilsmeier reagent. The method comprises the following steps: preparing a vilsmeier reagent by using N, N-dimethylformamide (DMF) and thionyl chloride (SOCl2), reacting the vilsmeier reagent with dicyclohexylurea (DCU), and carrying out aftertreatment to obtain the dicyclohexylcarbodiimide. According to the method, the vilsmeier reagent is adopted, the reaction can be carried out under mild conditions, the process is safe and stable, and the method is suitable for industrial large-scale production.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a method for preparing dicyclohexylcarbodiimide. Background technique [0002] Dicyclohexylcarbodiimide (DCC) is a biochemical dehydrating agent and polypeptide condensation agent, which is widely used in the synthesis of acids, anhydrides, aldehydes, ketones, polypeptides, and nucleic acids. In recent years. With the rapid development of bioengineering technology, the market demand for DCC is becoming more and more vigorous. [0003] The methods for synthesizing dicyclohexylcarbodiimide include thiourea method, urea method and phosgene method. The thiourea method uses cyclohexylamine as the starting material to form corresponding thiourea derivatives with carbon disulfide, and then removes hydrogen sulfide to convert it into DCC. The commonly used desulfurizers include mercuric oxide and sodium hypochlorite. [0004] Patent CN101096349A reports the preparation 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
IPC IPC(8): C07C267/00
CPCC07C257/10C07C267/00C07C2601/14
Inventor 崔宝龙梁寒冰王静王冠庆
Owner SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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