Mono-methylation method for amines compounds

An amine compound and monomethyl technology is applied in the field of monomethylation of amine compounds to achieve the effects of simple process route, high reaction conversion rate and easy separation

Inactive Publication Date: 2008-09-10
抚顺市化工研究设计院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Methanol and carbon dioxide, the direct by-products af

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1 is synthesized N-methylaniline by aniline

[0021] 93g of aniline, 90g of DMC, and 37g of diethylenetriamine were put into the autoclave, and after nitrogen replacement, the temperature was raised to 100°C, and the reaction was carried out for 12 hours. Then the low boiling point substances were distilled off, and the fraction at 194-196°C was collected to obtain 99g of N-methylaniline with a yield of 92.5%.

Embodiment 2

[0022] Embodiment 2 is synthesized N-methylformanilide by N-formanilide

[0023] Put 121 g of N-formanilide, 108 g of DMC, and 4.6 g of potassium carbonate into the reaction flask, raise the temperature to 90° C., and react under reflux for 6 hours. Then the low boiling point substances were distilled off, the product was distilled under reduced pressure, and the fraction at 130-133° C. / 2.1 kPa was collected to obtain 130 g of N-methylformanilide with a yield of 96.3%.

Embodiment 3

[0024] Embodiment 3 synthesizes N-methyl octadecylamine by octadecylamine

[0025] Put 269g of octadecylamine and 270g of DMC, 162g of methanol, and 3.5g of NaY molecular sieve into the autoclave, raise the temperature to 100°C, and react for 3 hours under the condition of natural pressure increase. Then the product was filtered and distilled to remove low boiling point substances, cooled and dried to obtain 269g of N-methylaniline with a yield of 95%.

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Abstract

The invention relates to the monomethylation of amine-group compounds, in particular to a monomethylation method for amine-group compounds. The method is characterized in that primary amine or secondary amine is used as materials, and methyl carbonate (DMC) is used as a methylation reagent. The method has the advantages that: due to high conversion rate of material amine-group compounds and high selectivity of monomethylation products, target monomethylation products are high in yield. The reaction liquid is kept basic all the time, and compared with other methods, the method can hardly cause the problem of the corrosion of equipments; the toxin of the reagent is light, the reaction condition is mild and the risk is small; the reaction can be completed in one step, the operational path is simple and easy to practice; products are easy to separate, and reaction byproducts of the main reaction are easy to process.

Description

technical field [0001] The present invention relates to the monomethylation of amine compounds, specifically using dimethyl carbonate (DMC) as a methylating agent, and finally a methyl group will be attached to the nitrogen atom of the amine compounds. Background technique [0002] As a large class of commonly used organic compounds, amine compounds are mostly used to react with methylating reagents to connect methyl groups, and formaldehyde and formic acid are also used to connect methyl groups through Eschweiler and W-Clarke reactions. of. However, the methylating reagents frequently used in the preceding methods refer to methyl halides (MeX; X=Cl, Br, I), dimethyl sulfate (DMS) and phosphoric acid esters, although they can be used under mild reaction conditions. Nitrogen atoms on methylated amines. However, these reagents have serious hidden dangers in terms of environment and operational safety. For example, dimethyl sulfate is a highly toxic compound, which is danger...

Claims

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Application Information

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IPC IPC(8): C07C209/60
Inventor 王庆
Owner 抚顺市化工研究设计院
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