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

A technology of imidazolidinediones and production methods, applied in the direction of organic chemistry, etc., can solve the problems of inability to realize industrialization, continuous production, inability to realize continuous production, cumbersome production procedures, etc., achieve conventional production equipment, reduce The production of three wastes and the effect of reducing production costs

Active Publication Date: 2022-03-11
ZHANGJIAGANG JIULI NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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.

Method used

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  • Continuous cycle industrial production method of 5-tert-butyl-5-hydroxy-1,3-diphenyl-2,4-imidazolidinone

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preparation example Construction

[0037] The device for preparing 5-tert-butyl-5-hydroxy-1,3-diphenyl-2,4-imidazolidinedione according to the present invention includes a Grignard reagent kettle 5, and the Grignard reagent kettle 5 passes through the pipeline It is connected to the Grignard reaction kettle 7, the quenching kettle 10 and the extraction kettle 12 in sequence, and the top of the quenching kettle 10 is connected to the distillation tower 16, the anhydrous calcium chloride drying tower 15 and the molecular sieve drying tower 14 in sequence through pipelines, and the distillation tower 16 The lower discharge port is connected to the discharge pipe 17, and the top of the molecular sieve drying tower 14 is connected to the Grignard reagent kettle 5 through a pipeline.

[0038] The feed inlet at the upper end of the Grignard reagent kettle 5 is connected to the tert-butyl chloride metering tank 1, the solvent tank 2, the low-pressure nitrogen delivery pipe 3, and the outlet of the magnesium scrap feedin...

Embodiment 1

[0046] The continuous cycle industrial production method of 5-tert-butyl-5-hydroxyl-1,3-diphenyl-2,4-imidazolidinedione described in Example 1 consists of the following steps:

[0047] (1) Preparation of Grignard reagent: under the protection of inert nitrogen gas and anhydrous conditions, the initiator of the prefabricated 5 liters of 1 mole per liter concentration is poured in 2000 liters of Grignard reagent kettle (conventional non-standard reaction kettle, volume 2 cubic, with the upper cover and neck about 2.3 cubic), then add 500 liters of anhydrous tetrahydrofuran and 15.6 kg of magnesium chips, slowly heat to 65 ° C to keep the reaction system slightly reflux, dropwise add tert-butyl chloride solution (52 kg of tert-butyl Chlorine is pre-dissolved in 500 liters of anhydrous tetrahydrofuran); the reaction is exothermic, and the slight reflux state in the kettle is maintained by adjusting the amount of heating steam in the reactor; after the dropwise addition, the reactio...

Embodiment 2

[0053] The continuous cycle industrial production method of 5-tert-butyl-5-hydroxyl-1,3-diphenyl-2,4-imidazolidinedione described in Example 2 consists of the following steps:

[0054] (1) Preparation of Grignard reagent: under the protection of inert nitrogen gas and anhydrous conditions, the initiator of the prefabricated 6.5 liters of 1 mole per liter concentration is poured in 2000 liters of Grignard reagent kettle (conventional non-standard reaction kettle, volume 2 cubic, plus the upper cover and neck about 2.3 cubic), then add 500 liters of anhydrous toluene and 14.9 kilograms of magnesium chips, slowly heat to 70 ° C to keep the reaction system slightly reflux, dropwise add tert-butyl chloride solution (52 kilograms of tert-butyl Chlorine is pre-dissolved in 500 liters of anhydrous toluene); the reaction is exothermic, and the slight reflux state in the kettle is maintained by adjusting the amount of heating steam in the reactor; after the dropwise addition, continue to...

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Abstract

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. Heat the initiator, solvent and magnesium chips to 65-75°C, add tert-butyl chloride dropwise to prepare the Grignard reagent, and then send the Grignard reagent to the Grignard reactor with 1,3-diphenyl-2,4 , 5-imidazolintrione is synthesized, the reaction solution generated by the reaction is transferred to a quenching kettle filled with dilute hydrochloric acid for quenching, and the reaction is separated to prepare 5-tert-butyl-5-hydroxyl-1 ,3‑Diphenyl‑2,4‑imidazolidinedione. The industrialized production method of the present invention creatively realizes the enlarged production of tert-butyl Grignard reagent, thereby realizing 5-tert-butyl-5-hydroxyl-1,3-diphenyl-2,4-imidazole The industrial continuous production of phenedione, and the purity and 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...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/66
Inventor 石卫民闫晗李润泽黄宝金苏旭
Owner ZHANGJIAGANG JIULI NEW MATERIAL TECH CO LTD
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