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Chemical synthesis of p-methoxyphenyl isocyanate

A technology of methoxyphenyl isocyanate and p-methoxyaniline, which is applied in the fields of pesticides, dyes, and synthetic medicines, can solve the problems of serious equipment corrosion, large safety hazards, and long reaction cycles, and achieve small equipment corrosion and safe and reliable production , the effect of low production cost

Inactive Publication Date: 2004-01-21
ZHEJIANG TONGFENG PHARMA & CHEM
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  • 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

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] P-methoxyaniline: bis(trichloromethyl) carbonate: toluene: 1,3-dimethyl-2-imidazolidinone=1: 0.35: 0.02 (molar ratio), the feeding amount of toluene is p-methoxy 8 times the mass of base aniline.

[0015] Add p-methoxyaniline, 1,3-dimethyl-2-imidazolidinone and toluene into the reaction kettle, after stirring evenly, add the toluene solution of bis(trichloromethyl)carbonate dropwise within 30 minutes at room temperature At the same time, open the absorption system of the by-product hydrogen chloride to industrial hydrochloric acid, and then heat up and reflux for 4 hours. (GC) 99.4%.

Embodiment 2

[0017] P-methoxyaniline: bis(trichloromethyl) carbonate: 1,3-dimethyl-2-imidazolidinone=1: 0.35: 0.01 (molar ratio), the charging capacity of reclaiming toluene is p-methoxy 8 times the mass of aniline.

[0018] Add p-methoxyaniline, 1,3-dimethyl-2-imidazolidinone and recovered toluene into the reaction kettle, after stirring evenly, add bis(trichloromethyl)carbonate toluene dropwise within 30 minutes at room temperature Solution, simultaneously open the absorption system for producing industrial hydrochloric acid by-product hydrogen chloride, then heat up and reflux for 4 hours, after the reaction is completed, first atmospheric distillation recovers toluene, then vacuum distillation, and collects the fraction at 106-108°C under 2KPa, with a yield of 96.3%. Content (GC) 99.3%.

Embodiment 3

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

[0021] Feed and react according to Example 1, and finally collect the fraction at 106-108° C. under 2 KPa, with a yield of 97.0% and a content (GC) of 99.0%.

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PUM

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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, pesticide and dyestuff, and mainly relates to a chemical synthesis method of p-methoxyphenyl isocyanate. Background technique [0002] P-methoxyphenyl isocyanate is an important intermediate of medicine, pesticide and polymer material. In the prior art, the 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 in the world, which has great potential safety hazards, and the reaction cycle is long, and the equipment is seriously corroded. The most troublesome thing is that the amount of three wastes is large, and the treatment is difficult and expensive. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a chemical synt...

Claims

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Application Information

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IPC IPC(8): C07C263/06C07C265/12
Inventor 蔡戈冬曹国君王波华
Owner ZHEJIANG TONGFENG PHARMA & CHEM
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