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Production process of imidazole aldehyde

A production process and imidazolaldehyde technology are applied in the production technology field of imidazolyl, can solve the problems of long cycle, high cost, unfavorable promotion and industrialized production, etc., achieve good stability, reduce by-products, optimize reaction conditions and feed ratio Effect

Inactive Publication Date: 2019-06-28
江西三元药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method only requires two steps of reaction, the raw material reagents need to be purchased by entrustment, which has a long cycle and high cost, which is not conducive to popularization and industrial production.

Method used

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  • Production process of imidazole aldehyde
  • Production process of imidazole aldehyde
  • Production process of imidazole aldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Put 500kg of valeronitrile and 300kg of methanol into the esterification kettle, then cool down to 0°C, and feed 280kg of hydrogen chloride gas (prepared by mixing phosphorus trichloride and hydrochloric acid solution according to the mass ratio of 2.0:1.65, and control the pressure in the kettle to be lower than 0.1MPa, The temperature is 7-9°C for reaction), after the aeration, keep the temperature at 10°C for 15h, add 200L of sodium hydroxide solution with a mass fraction of 30%, control the temperature below 10°C for 5h to obtain imidate, add 230kg of toluene, Extract to obtain imidate toluene solution; add 250kg of glycine, 750kg of methanol, control the temperature at 20°C for 3h, control the temperature below 55°C and the pressure at -0.01Mpa for vacuum distillation, and then carry out vacuum distillation at 55°C and -0.01MPa Bake for 3 hours to obtain imidic acid; put it into the hydroformylation kettle, add 550kg of phosphorus oxychloride, 200kg of toluene, cont...

Embodiment 2

[0052] Put 500kg of valeronitrile and 270kg of methanol into the esterification kettle, then cool down to 5°C, and feed 280kg of hydrogen chloride gas (prepared by mixing phosphorus trichloride and hydrochloric acid solution according to the mass ratio of 2.0:1.65, and control the pressure in the kettle to be lower than 0.1MPa, The temperature is 7-9°C for reaction), after the aeration, keep the temperature at 12°C for 12h, add 250L of sodium hydroxide solution with a mass fraction of 30%, control the temperature below 10°C for 8h to obtain imidate, add 250kg of toluene, Extract to obtain imidate toluene solution; add 300kg of glycine, 750kg of methanol, control the temperature at 25°C for 2h, control the temperature below 55°C and the pressure at -0.01Mpa to carry out vacuum distillation, and then at 55°C and -0.01MPa Bake for 3 hours to obtain imidic acid; put it into the hydroformylation kettle, add 660kg of phosphorus oxychloride, 250kg of toluene, add 375kg of N,N-dimethyl...

Embodiment 3

[0055] Put 500kg of valeronitrile and 280kg of methanol into the esterification tank, then lower the temperature to 2°C, and feed 280kg of hydrogen chloride gas (prepared by mixing phosphorus trichloride and hydrochloric acid solution according to the mass ratio of 2.0:1.65, and control the pressure in the tank to be lower than 0.1MPa, The temperature is 7-9°C for reaction), after the aeration, keep the temperature at 12°C for 15h, add 250L of sodium hydroxide solution with a mass fraction of 30%, control the temperature below 10°C for 8h to obtain imidate, add 250kg of toluene, Extract to obtain imidate toluene solution; add 260kg of glycine, 750kg of methanol, control the temperature at 25°C for 3h, control the temperature below 55°C and the pressure at -0.01Mpa for vacuum distillation, and then conduct vacuum distillation at 55°C and -0.01MPa Bake for 3 hours to obtain imidic acid; put it into the hydroformylation kettle, add 550kg of phosphorus oxychloride, 220kg of toluene...

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Abstract

The invention provides a production process of imidazole aldehyde. Imiline is prepared by using valeronitrile and methanol as raw materials, glycine and methanol are added to prepare imidic acid, anda further reaction is conducted with phosphorus oxychloride and DMF to obtain the imidazole aldehyde. By controlling reaction conditions and the feed ratio of the raw materials, the formation of by-products is reduced, and the yield is improved. A decoking and decolorization reaction and an activated carbon decolorization reaction are adopted, the solubility change of the imidazole aldehyde underdifferent pH conditions is used for purifying a product, and finally, the imidazole aldehyde with a purity of more than 99.2% is obtained by recrystallization.

Description

technical field [0001] The invention belongs to the technical field of chemical intermediate synthesis, and in particular relates to a production process of imidazole aldehyde. Background technique [0002] Imidazole aldehyde, 2-butyl-5-chloro-1H-imidazole-4-carbaldehyde is a heterocyclic compound and an important intermediate in the synthesis of sartan antihypertensive drugs. [0003] Generally, the production process of imidazole aldehyde can be classified according to the difference of some raw materials in the reaction process, and can be divided into dihydroxyacetone method, methyl glycine method and glycine method and so on. The dihydroxyacetone method refers to the use of valeronitrile as a raw material to react with methanol and hydrogen chloride gas to form pentamidine hydrochloride, which is then directly condensed with dihydroxyacetone in liquid ammonia under heat and pressure, and then further reacted The imidazole aldehyde is obtained. The process conditions a...

Claims

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Application Information

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IPC IPC(8): C07D233/68
Inventor 葛国华吴卫红涂军华李蒋健张成龙孙小冬
Owner 江西三元药业有限公司
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