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Preparation method of 2-n-butyl-4-chloro-5-formyl imidazole

A technology of formyl imidazole and methyl imidazole, which is applied in the field of preparation of 2-n-butyl-4-chloro-5-formyl imidazole, can solve the problems of difficult mixing, unsatisfactory flow state, low reaction rate and the like, and achieves The effect of improving flow state, fast and uniform mixing reaction, and improving reaction efficiency

Pending Publication Date: 2021-01-15
ZHEJIANG HUADEE DYESTUFF CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to make up for the deficiencies of the prior art and solve the need of the existing 2-n-butyl-4-chloro-5 formyl imidazole in the production process, by adding the material dropwise into the reactor, it is difficult for the upper material to react with the lower layer The solvent is quickly and uniformly mixed, and the flow state in the reactor is not ideal, resulting in the problem that the actual reaction rate is not high. A kind of preparation method of 2-n-butyl-4-chloro-5-formyl imidazole proposed by the present invention

Method used

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  • Preparation method of 2-n-butyl-4-chloro-5-formyl imidazole

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preparation example Construction

[0031] Such as Figure 1 to Figure 7 Shown, a kind of preparation method of 2-n-butyl-4-chloro-5-formyl imidazole comprises the following steps:

[0032] S1, cyclization of valeraldehyde and methylglyoxal to obtain 2-butyl-5-methylimidazole;

[0033] S2. Add the 2-butyl-5 methylimidazole obtained in step S1 to the reaction kettle through the addition pipe, add the chlorination reagent to the reaction kettle through the second feed pipe 6, and add water and catalyst, and stir evenly. Synthesis of 2-butyl-4-chloro-5-methylimidazole under the action of chlorination reagent, the reaction temperature is 35-40°C, and the reaction time is 6-10 hours;

[0034] S3. Add sodium persulfate in batches to the 2-butyl-4-chloro-5-methylimidazole obtained in step S2 through the first feed pipe 5, heat up to 50-55°C and react for 3-5 hours to obtain 2-n-Butyl-4-chloro-5-formyl imidazole;

[0035] Wherein, the reaction kettle includes a kettle body 1, the upper end of the kettle body 1 is pro...

Embodiment approach

[0037] As an embodiment of the present invention, the spiral stirring plate 14 is provided with a plurality of radially arranged chute 15 at intervals, and the inner wall of the chute 15 is fixedly provided with a second rod 24 extending outward, The second rod 24 is covered with a second magnetic block 26 that can slide along its extension direction, and the second magnetic block 26 is connected to the inner wall of the chute 15 through a second spring 25, and the second spring 25 Set outside the second pole 24. Through the setting of the chute 15, a part of the material flowing up along the upper surface of the spiral stirring plate 14 can be intercepted, and part of the material in the chute 15 moves outward along the chute 15 to participate in the mixing between the materials on the periphery of the spiral stirring plate 14 At the same time, part of the material stays in the chute 15 and mixes with the subsequent intercepted material, thus improving the effect and efficien...

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Abstract

The invention relates to the technical field of chemical production, in particular to a preparation method of 2-n-butyl-4-chloro-5-formyl imidazole. A reaction kettle used in the method comprises a kettle body, an upper cover is arranged at the upper end of the kettle body, and an adding pipe communicated with an inner cavity of the kettle body is arranged on one side of the upper cover; a base isfixedly arranged at the lower end of the kettle body, a discharge pipe communicated with an inner cavity of the kettle body is arranged at the lower end of the kettle body, the discharge pipe penetrates through the base and extends to one side of the base, and an on-off valve is arranged on the discharge pipe. Through the arrangement of the spiral stirring plate, the transition cavity and the through holes, materials in the kettle body can be disturbed in the vertical plane and the horizontal plane, the reaction efficiency is improved, and meanwhile, an added chlorination reagent or sodium persulfate can be directly guided to different layers in the kettle body, so that the added chlorination reagent or sodium persulfate can be mixed and reacted with the materials more quickly and uniformly; and the mixing efficiency is quickened.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a preparation method of 2-n-butyl-4-chloro-5-formyl imidazole. Background technique [0002] 2-n-butyl-4-chloro-5-formyl imidazole is a key intermediate of the drug losartan, and the general synthesis method of 2-n-butyl-4-chloro-5-formyl imidazole uses valeronitrile as the starting material , first react to form amidine, and then synthesized by chlorination and acylation. [0003] Chinese patent (application number: 2017103002498) discloses a preparation method of 2-n-butyl-4-chloro-5-formyl imidazole, which starts with pentamidine hydrochloride and glycine tert-butyl ester hydrochloride Reaction of raw materials to obtain (1-iminopentyl)glycine tert-butyl ester, and then deprotection, ring closure, chlorination and vilsemier reaction, and recrystallization to obtain 2-n-butyl-4-chloro-5-formyl imidazole. The raw materials of this method are cheap and easy to obtai...

Claims

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Application Information

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IPC IPC(8): C07D233/68
CPCC07D233/68
Inventor 顾敏伟
Owner ZHEJIANG HUADEE DYESTUFF CHEM
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