Process for preparing carbamate, urea and their derivatives as well as 2-oxzolidone

A technology of carbamate and oxazolidinone is applied in the field of preparing nitrogen-containing carbonyl compounds, which can solve the problems of equipment corrosion, difficulty, and increase the cost of catalyst use, and achieves mild reaction conditions, high product selectivity, and catalyst system. simple effect

Inactive Publication Date: 2007-01-24
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods cause a large amount of chlorine and bromine plasma in the reaction liquid, which can easily cause corrosion of equipment under high temperature and high pressure conditions, and are used as cocat...

Method used

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  • Process for preparing carbamate, urea and their derivatives as well as 2-oxzolidone
  • Process for preparing carbamate, urea and their derivatives as well as 2-oxzolidone
  • Process for preparing carbamate, urea and their derivatives as well as 2-oxzolidone

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Experimental program
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Effect test

Embodiment 1

[0031]

[0032] In a 100 milliliter autoclave, add palladium acetate 0.005mmol and cocatalyst 1,3-dimethyl-imidazolium iodide (MMImI) 0.02mmol successively, then add 50mmol amine compounds and 10 milliliters of ethylene glycol dimethylamine reaction solvent , airtight reaction kettle; the pressure of filling oxygen is 0.5Mpa and the pressure of carbon monoxide is 3.5MPa, and reacting for a certain period of time under the condition of reaction temperature of 120°C. After the reaction, cool to room temperature and unload the kettle; the reaction solution precipitates white needle-shaped product N, N'-diphenylurea (2a) at low temperature, and is filtered and weighed to calculate the yield. After qualitative and quantitative analysis by 6890 / 5973 chromatography-mass spectrometry, high-performance liquid chromatography, and nuclear magnetic resonance, the purity of the product is greater than 99%, and the separation yield can reach 96%.

Embodiment 2

[0034] The cocatalyst used is 1-methyl-3-butyl-imidazolium iodide (BMImI), and the remaining reaction conditions are the same as in Example 1; the isolated yield is 98%, and the selectivity is greater than 99%.

Embodiment 3

[0036]The metal catalyst used is palladium carbon, and the remaining reaction conditions are the same as in Example 1; the separation yield is 95%, and the selectivity is greater than 99%.

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Abstract

The present invention discloses preparation of nitrogen containing carbonyl compound, and is especially the process of preparing carbamate, urea and their derivatives as well as 2-oxazolidone through oxidizing and carbonylating organic amine compound in the presence of one kind of multifunctional catalyst. By using salt of VIII metal and Cu as main metal catalyst and the ionic solution of halogenated pyridine salt, quaternary ammonium salt or quaternary phosphate salt as co-catalyst and through oxidizing and carbonylating organic amine compound, carbamate, urea and their derivatives as well as 2-oxazolidone may be prepared at oxygen pressure of 0.2-1.0 MPa, CO pressure of 1.0-4.0 MPa, reaction temperature of 80-220 deg.c, and in reaction time of 0.5-4 hr. Compared with the technological process adopting traditional catalyst, the present invention has the advantages of simple system, easy preparation, mild reaction condition and high selectivity.

Description

technical field [0001] The invention relates to a method for preparing nitrogen-containing carbonyl compounds, in particular to the preparation of carbamate, urea and its derivatives and 2-oxazolidinone by selecting a multifunctional catalyst and oxidative carbonylation of organic amine compounds method. Background technique [0002] Urethane, urea and its derivatives, and 2-oxazolidinone are a class of nitrogen-containing carbonyl compounds and are important fine chemical intermediates. When the organic amines are prepared by oxidative carbonylation, due to the difference in the selected catalysts and process operating conditions, their production and preparation have received extensive attention. [0003] Hirai (USP 4170708), Scholl (USP 4490551) and Moy (USP 4242520; 4258201) and others successively used selenium, sulfur, and tellurium as catalysts to prepare urea and carbamate by oxidative carbonylation of amine compounds. Zajacek et al. (USP3956360) disclosed a method...

Claims

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Application Information

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IPC IPC(8): C07C269/04C07C271/06C07C273/02C07C273/18C07D263/22C07B41/06
Inventor 夏春谷李福伟彭新高胡斌
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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