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

Chemical synthesis of p-methoxyphenyl isocyanate

A technology of methoxybenzene isocyanate and p-methoxyaniline is applied in the fields of pesticides, dyes, and synthetic medicines, and can solve the problems of serious equipment corrosion, long reaction period, and large safety hazards, and achieves low equipment corrosion and low production cost. , the production of safe and reliable results

Inactive Publication Date: 2005-11-23
ZHEJIANG TONGFENG PHARMA & CHEM
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this process is that it uses phosgene, a highly toxic raw material that is restricted in the world, which has great safety hazards, and the reaction cycle is long, and the equipment is severely corroded. The most troublesome thing is that the amount of three wastes is large, and the treatment is difficult and expensive

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
  • Chemical synthesis of p-methoxyphenyl isocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] P-anisidine: bis(trichloromethyl) carbonate: 1,3-dimethyl-2-imidazolidinone=1:0.35:0.02, the feed amount of toluene is 8 times the mass of p-anis .

[0015] P-Methoxyaniline, 1,3-dimethyl-2-imidazolidinone and toluene are added to the reaction kettle, after stirring, add bis(trichloromethyl) carbonate toluene dropwise within 30 minutes at room temperature At the same time, open the absorption system of the by-product hydrogen chloride to produce industrial hydrochloric acid, and then heat and reflux for 4 hours. After the reaction is completed, the toluene is recovered by atmospheric distillation, and then vacuum distillation. The fraction at 106-108°C is collected under 2000 Pascals. The yield is 95.6 %, content (GC) 99.4%.

Embodiment 2

[0017] P-anisidine: bis(trichloromethyl) carbonate: 1,3-dimethyl-2-imidazolidinone=1:0.35:0.01, the amount of toluene recovered is 8 of the mass of p-anis Times.

[0018] P-methoxyaniline, 1,3-dimethyl-2-imidazolidinone and recycled toluene were added to the reaction kettle, and after stirring uniformly, bis(trichloromethyl) carbonate was added dropwise within 30 minutes at room temperature. Toluene solution, and open the absorption system of the by-product hydrogen chloride to produce industrial hydrochloric acid at the same time, and then the reaction is heated and refluxed for 4 hours. After the reaction is completed, the toluene is recovered by atmospheric distillation, and then vacuum distillation. The fraction at 106-108°C is collected at 2000 Pascals. Yield 96.3%, content (GC) 99.3%.

Embodiment 3

[0020] P-methoxyaniline: bis(trichloromethyl) carbonate: 1,3-dimethyl-2-imidazolidinone = 1:0.50:0.02, the feeding amount of toluene is 8 times the mass of p-anisidine .

[0021] According to the feeding reaction in Example 1, the fraction at 106-108°C was collected at 2000 Pascals, with a yield of 97.0% and a content (GC) of 99.0%.

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 chemical synthesis of p-methoxyphenyl isocyanate is one process inside organic solvent with methoxyphenyl amine and di(trichloromethyl) carbonate as material and in the presence of catalyst. The process has the material molar ratio of methoxyphenyl amine to di(trichloromethyl) carbonate to catalyst being 1 to 0.34-0.8 to 0.01-0.1; organic solvent amount is 3-12 times mass of methoxyphenyl amine; the reaction temperature is 20-180 deg.c and reaction period is 4-10 hr. The organic solvent may be benzene, toluene, xylene, chlorobenzene, dichloro benzene, dichloro methane, trichloro methane, carbon tetrachloride, ethylidene dichloride, tetrafuran or hexaalkane epoxide. The said process uses no virulent phosgene and diphosgene, and is safe, reliable, high in yield, low in cost, and less corrosive and waste exhaust.

Description

Technical field [0001] The invention relates to the field of synthetic medicine, pesticides and dyes, and is mainly a chemical synthesis method of p-methoxyphenyl isocyanate. Background technique [0002] P-methoxyphenyl isocyanate is an important intermediate of medicine, pesticide and polymer material. The prior art chemical synthesis method of p-methoxyphenyl isocyanate is prepared by reacting phosgene and p-methoxyaniline as raw materials. The disadvantage of this process is that it uses phosgene, a highly toxic raw material that is restricted internationally, and has high potential safety hazards. It also has a long reaction cycle and serious equipment corrosion. The most troublesome is the large amount of three wastes, and the processing is difficult and expensive. Summary of the invention [0003] The technical problem to be solved by the present invention is to provide a p-methoxyphenyl isocyanate chemical synthesis method with reaso...

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): C07C263/06C07C265/12
Inventor 蔡戈冬曹国君王波华
Owner ZHEJIANG TONGFENG PHARMA & 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