Continuous circulation industrial production method of 5-tert-butyl-5-hydroxy-1, 3-diphenyl-2, 4-imidazolinedione

Abstract

The invention belongs to the technical field of intermediate preparation, and particularly relates to a continuous circulation industrial production method of 5-tert-butyl-5-hydroxy-1, 3-diphenyl-2, 4-imidazolinedione. The method comprises the following steps: heating an initiator, a solvent and magnesium chips to 65-75 DEG C, dropwise adding tert-butyl chloride to prepare a Grignard reagent, then conveying the Grignard reagent to a Grignard reaction kettle, carrying out a synthetic reaction on the Grignard reagent and 1, 3-diphenyl-2, 4, 5-imidazolintrione, transferring a reaction solution generated by the reaction to a quenching kettle containing diluted hydrochloric acid for quenching, separating the solution after the reaction is finished, and preparing 5-tert-butyl-5-hydroxy-1, 3-diphenyl-2, 4-imidazolidinone According to the industrial production method disclosed by the invention, the amplification production of the tert-butyl Grignard reagent is creatively realized, so that the industrial continuous production of the 5-tert-butyl-5-hydroxy-1, 3-diphenyl-2, 4-imidazoline diketone is realized, and the purity and the yield of the prepared product are high.

Description

technical field [0001] The invention belongs to the technical field of intermediate preparation, and in particular relates to a continuous cycle industrial production method of 5-tert-butyl-5-hydroxyl-1,3-diphenyl-2,4-imidazolidinedione. Background technique [0002] Triazone is the raw material for the synthesis of the herbicide metrizone, and 3,3-dimethyl-2-oxo-butyric acid is an irreplaceable important intermediate in the synthesis of triazone, 3,3-dimethyl The synthesis of -2-oxo-butyric acid is obtained by hydrolysis and acidification of 5-tert-butyl-5-hydroxy-1,3-diphenyl-2,4-imidazolidinedione. Patent CN 2019102434671 discloses a method for preparing 3,3-dimethyl-2-oxo-butyric acid, in which oxalyl chloride is contacted with N,N'-diphenylurea to obtain 1,3-diphenyl Base-2,4,5-imidazolintrione; The 1,3-diphenyl-2,4,5-imidazolintrione is reacted with a Grignard reagent containing tert-butyl to obtain 5- tert-butyl-5-hydroxy-1,3-diphenyl-2,4-imidazolidinedione; the res...

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Problems solved by technology

In addition to the target intermediate, the organic phase also contains a large amount of solvent, resulting in waste of solvent, and the preparation method is under laboratory conditions, which cannot realize industrialization and continuous production

[0005] Moreover, the production process of 5-tert-butyl-5-hydroxy-1,3-diphenyl-2,4-imidazolidinedione disclosed in the prior art is cumbersome, and continuous and industrialized production cannot be realized. It is only a laboratory Therefore, it is necessary to explore a set of methods that can be applied to industrial production. On the premise of overcoming the above difficulties, simplify the production process, reduce the generation of waste water and waste gas, and maximize the use of raw materials.

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