A kind of preparation method of n-formamide compounds

A technology for formamides and compounds, which is applied in the field of preparation of N-formamides, can solve the problems of difficult reuse of catalysts, need heavy metal catalysts, complex reaction systems and the like, and achieves low cost, high selectivity and simple process. Effect

Active Publication Date: 2018-06-08
HUIZHOU RES INST OF SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The purpose of the present invention is to provide a solution for the problems of heavy metal catalysts, inert gas atmosphere, complex reaction system, high temperature and pressure, difficult separation of products and difficult reuse of catalysts in the existing synthetic routes of N-formamide compounds. A kind of preparation method of N-formamide compound

Method used

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  • A kind of preparation method of n-formamide compounds
  • A kind of preparation method of n-formamide compounds
  • A kind of preparation method of n-formamide compounds

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Experimental program
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Effect test

Embodiment 1

[0035] In the 10mL stainless steel autoclave, add the catalyst of 0.001mmol (M is Zn in the general formula (1), R 1 , R 2 , R 3 are all hydrogen groups) and 0.001mmol cocatalyst (R in general formula (2) 4 is n-butyl), 1mmo N-methylaniline and 1mmol phenylsilane are used as raw materials, the carbon dioxide pressure is adjusted to 0.5MPa, and the stirring reaction is carried out at a temperature of 25°C for 15h. After the reaction is completed, ether is added to centrifuge to recover the catalyst. The solvent was removed by rotary evaporation, and the product N-methylformanilide was obtained after vacuum drying with a yield of 95%.

Embodiment 2

[0037] In the 10mL stainless steel autoclave, add the catalyst of 0.001mmol (M is Al in the general formula (1), R 1 , R 2 , R 3 are all hydrogen groups) and 0.001mmol cocatalyst (R in general formula (2) 4 n-butyl), 1mmo N-methylaniline and 1mmol phenylsilane are used as raw materials, the carbon dioxide pressure is adjusted to 5MPa, and the stirring reaction is carried out at a temperature of 100°C for 3h. After the reaction, ethyl acetate is added to centrifuge to recover the catalyst. The solvent was removed from the clear liquid by rotary evaporation, and the product N-methylformanilide was obtained after vacuum drying with a yield of 99%.

Embodiment 3

[0039] In the 10mL stainless steel autoclave, add the catalyst of 0.001mmol (M is Co in the general formula (1), R 1 and R 3 are all hydrogen groups, R 2 is methyl) and 0.001mmol cocatalyst (R in general formula (2) 4 is n-butyl), 1mmol 2-methoxy-N-methylaniline and 1mmol diphenylsilane are used as raw materials, the pressure of carbon dioxide is adjusted to 1MPa, and the stirring reaction is carried out at a temperature of 60°C for 6h. After the reaction is completed, add two Methane chloride was centrifuged to recover the catalyst, the supernatant liquid was removed by rotary evaporation, and the product 2-methoxy-N-methylformanilide was obtained after vacuum drying with a yield of 97%.

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Abstract

The invention discloses a preparation method of N-formamide compounds. Carbon dioxide and organic amines are used as raw materials, hydrogen-containing silane is added as a reducing agent, and a 0.1-1.0 mol% salen-type metal complex is used as a catalyst. Under the conditions of 0.1-5.0 MPa and a temperature of 25-100 ° C, with or without adding a co-catalyst, synthesize N-formamide organic compounds; after the reaction, add an organic solvent, centrifuge, separate the catalyst, and pass the supernatant through After the solvent is removed by rotary evaporation, N-formamide compounds are obtained. The preparation method has the advantages of mild reaction conditions, no need to add any organic solvent, simple operation, high catalytic activity, good substrate compatibility, etc., conforms to a green synthesis process, and is suitable for industrial production. In addition, the catalytic system provided by the present invention can be conveniently separated from the reaction system by adding a solvent, so as to realize the recycling of the catalyst.

Description

technical field [0001] The invention relates to the technical field of green chemistry, in particular to a preparation method of N-formamide compounds. Background technique [0002] With the intensification of the global warming effect and the development of organic chemistry, many scientific researchers will CO 2 As an environmentally friendly and cheap and readily available C1 resource, it is converted into various high value-added chemicals through chemical reactions. Among them, the green chemistry of obtaining formamide through carbon dioxide instead of toxic carbon monoxide has attracted the attention of chemists. [0003] Hydrogen is the most atom-economical reducing agent for reducing carbon dioxide, but harsh reaction conditions, such as high pressure and high reaction temperature of the gas mixture, prevent the widespread application of hydrogen. In addition, the source of hydrogen limits the industrial application of the reaction. However, cheap and non-toxic h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/185C07C231/10C07C233/05C07C233/18C07C233/15B01J31/22
CPCY02P20/582Y02P20/584
Inventor 纪红兵林小微罗荣昌周贤太
Owner HUIZHOU RES INST OF SUN YAT SEN UNIV
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