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Method for preparing 1-methylimidazole

A technology of methyl imidazole and methylamine, applied in the field of chemical synthesis, can solve the problems of high amine dosage and low yield, and achieve the effects of improving yield, reducing production cost and reducing dosage

Inactive Publication Date: 2017-02-22
JIANGSU CALE NEW MATERIALS
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The technical problem to be solved in the present invention is to provide a method for preparing 1-methylimidazole to solve the problems of lower yield and higher amine consumption in the prior art.

Method used

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  • Method for preparing 1-methylimidazole

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Experimental program
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Effect test

Embodiment 1

[0024] Drop into 40% 1-methylamine 280g and 20% ammoniacal liquor 300g and 40g ammonium bicarbonate in the three-necked flask of 2L, water-bath is warmed up to 40~45 ℃, drop by 40% glyoxal 500g and 37% 278g of formaldehyde is configured as a mixed aldehyde. After the dropwise addition is completed, it is raised to 50°C for 2 hours. After the heat preservation is completed, the reaction solution is concentrated and then rectified. Under a vacuum of 4.0KPa, collect 100 ~ The fraction at 110°C yielded 220 g of 1-methylimidazole, with a yield of 78%.

Embodiment 2

[0026] Drop into 40% 1-methylamine 280g and 20% ammoniacal liquor 300g and 25g ammonium carbonate in the three-necked flask of 2L, water-bath is warming up to 40~45 ℃, drop by 40% glyoxal 500g and 37 % of 278g of formaldehyde is configured as a mixed aldehyde. After the dropwise addition is completed, it is raised to 50°C for 2 hours. After the heat preservation is completed, the reaction solution is concentrated and then rectified. Under a vacuum of 4.0KPa, collect 100-110 ℃ fraction, 225g of 1-methylimidazole product was obtained, and the yield was 79.7%.

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Abstract

The invention discloses a method for preparing 1-methylimidazole. The method comprises the steps of mixing a water solution of 1-methylamine, ammonia water and ammonium carbonate, then, carrying out heating, adding mixed aldehyde into the heated mixture, and then, carrying out a reaction; and after the reaction is completed, subjecting the obtained reaction solution to concentration and rectification, thereby preparing 1-methylimidazole. Compared with the prior art, the method has the advantages that 1-methylimidazole is synthesized in one step by adopting the traditional mixed aldehyde cyclization method, ammonium carbonate is adopted to replace part of ammonia water and serves as a reaction accelerant, meanwhile, the consumption of 1-methylamine and ammonia water can be lowered, and the production cost is reduced. Meanwhile, after ammonium carbonate is used, the yield of the method can be increased by 10% compared with that of the traditional synthesis methods.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for preparing 1-methylimidazole. Background technique [0002] Imidazole derivatives are widely used in medicine, pesticides and materials. In recent years, the application of imidazole derivatives in materials has shown a rapid development trend, especially the representative 1-methylimidazole has a unique application. For example, 1-methylimidazole is used as an additive in the exploitation of shale gas in foreign countries. Its traditional synthetic method includes a one-step cyclization method and imidazole substitution method, wherein the one-step cyclization method mainly adopts the synthetic method of mixed aldehydes (glyoxal and formaldehyde), ammonia water and 1-methylamine, but its traditional synthetic method includes The rate is low, it is reported that in M.R.Grimmett, adv.Heterocycl.Chem, v12, p 1 (1970), formaldehyde and ammonium carbonate, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/58
CPCC07D233/58
Inventor 王扣军谢韦殷勇
Owner JIANGSU CALE NEW MATERIALS
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