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Method for synthesizing carbanilate by the reaction of aniline, urea and alcohol

A technology for the synthesis of phenylcarbamate and alcohol, which is applied in the preparation of carbamic acid derivatives, chemical instruments and methods, and the preparation of organic compounds. Mild, highly selective effect

Inactive Publication Date: 2004-11-17
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the technological researches starting from urea focus on the synthesis of dimethyl carbonate, and the research report on the synthesis of phenylcarbamate by the reaction of aniline, urea and alcohol has not been seen so far.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 0.1 mol of aniline, 0.08 mol of urea, 0.5 mol of methanol and 0.06 mol of HZSM5 were added to a 150 ml autoclave with electromagnetic stirring and an automatic temperature control system. After vacuuming with nitrogen, the autoclave was heated to 160° C. with stirring at a heating rate of 4° C. / min, and reacted for 4 hours. After 4 hours, the autoclave was cooled and a sample was taken for GC analysis. Results: The conversion rate was 15%, and the selectivity was 86%.

Embodiment 2

[0019] In a 150ml autoclave with electromagnetic stirring and automatic temperature control system, add 0.1mol of aniline, 0.12mol of urea, 0.6mol of n-propanol, and 0.08mol of Pd / C. After vacuuming with nitrogen, the autoclave was heated to 180° C. with stirring at a heating rate of 6° C. / min, and reacted for 3 hours. After 3 hours, the autoclave was cooled and a sample was taken for GC analysis. Results: The conversion rate was 12%, and the selectivity was 78%.

Embodiment 3

[0021] In a 150ml autoclave with electromagnetic stirring and automatic temperature control system, add 0.1mol of aniline, 0.1mol of urea, 0.4mol of ethanol, 0.04mol of ZnCl 2 . After vacuuming with nitrogen, the autoclave was heated to 150° C. with stirring at a heating rate of 10° C. / min, and reacted for 5 hours. After 5 hours, the autoclave was cooled and a sample was taken for GC analysis. Results: The conversion rate was 17%, and the selectivity was 65%.

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Abstract

A process for synthesizing benzene carbamic acid ester from phenylamine, urea and alcohol by charging a finite amount of catalyst at suitable reaction temperature and reaction time, reacting phenylamine with urea. The advantages of the invention are mild reaction condition, simple operation process, easy available catalyst, good raw material economy and high reaction selectivity.

Description

technical field [0001] The invention belongs to a method for synthesizing phenylcarbamate, in particular to a method for synthesizing phenylcarbamate through a non-phosgene route. Background technique [0002] Isocyanate is an important organic synthesis intermediate and the main raw material for polyurethane synthesis, which can be widely used in polymer materials such as polyurethane, coatings, dyes and pesticides. The isocyanate product series mainly include TDI (toluene diisocyanate), MDI (4,4-diphenylmethane diisocyanate), PI (phenyl isocyanate) and so on. According to statistics, the current demand for TDI and MDI in the world is growing at a rate of 5.5% and 8% per year, and the demand in my country is growing at a rate of 7% and 10% to 12% per year. In the traditional isocyanate synthesis process, most products are synthesized by phosgene method. This synthesis process has disadvantages such as long route, high cost, highly toxic raw materials, corrosion of equipme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C269/04C07C271/06
Inventor 王心葵彭少逸李其峰亢茂青王军威董文生
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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