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Synthetic method of benzoxazolinone

A benzoxazolone and synthetic method technology, applied in the direction of organic chemistry, can solve the problems of reducing operating procedures, unfavorable environmental protection, etc., and achieve the effects of uniform heating, easy handling, and simple post-processing

Active Publication Date: 2020-01-17
湖南速博生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The present invention mainly aims at overcoming the problem that the organic solvent system used in the traditional synthesis process of benzoxazolone is not conducive to environmental protection, etc., and provides a continuous synthesis method of benzoxazolone with a solvent-free system. The reaction conditions of the method are mild, and the equipment is The corrosiveness is small; the post-treatment is simple, just transfer the reaction solution to hot water, cool and crystallize, filter, and dry, the reaction and post-treatment are continuous, reducing the operating procedures, and because no organic solvent is used in the reaction system, The waste generated in industrial production is also greatly reduced, making the whole process more green and environmentally friendly

Method used

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  • Synthetic method of benzoxazolinone
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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The 2000mL horizontal double-helix reactor controls the rotation speed, the system is under negative pressure (relative vacuum is -0.02MPa), the temperature is raised to 120°C, and 660.0g (6.05mol) of 2-aminophenol and 399.6g (6.66mol) of urea It is continuously fed into the horizontal double-helix reactor in proportion, the average residence time of the molten material in the reactor is 1h, and the ammonia gas generated is removed from the system in time. The reaction material was transferred to 1320.0g of 90°C water while it was hot, and after continuing to stir for 30min, cooled to 30°C, filtered and dried to obtain 795.1g of benzoxazolone with a content of 99.1% (external standard of liquid chromatography), yield It is 97.3% (based on 2-aminophenol).

Embodiment 2

[0033] The 2000mL horizontal double-helix reactor controls the rotation speed, the system is under negative pressure (relative vacuum degree is -0.01MPa), the temperature is raised to 150°C, and 660.0g (6.05mol) of 2-aminophenol and 435.9g (7.26mol) of urea It is continuously fed into the horizontal double-helix reactor in proportion, the average residence time of the molten material in the reactor is 0.5h, and the ammonia gas generated is removed from the system in time. The reaction material was transferred to 660.0g of 50°C water while it was hot, and after continuing to stir for 30min, cooled to 20°C, filtered and dried to obtain 803.3g of benzoxazolone with a content of 98.7% (external standard of liquid chromatography), yield It is 98.3% (based on 2-aminophenol).

Embodiment 3

[0035] The 2000mL horizontal double-helix reactor controls the rotation speed, the system is under negative pressure (relative vacuum is -0.01MPa), the temperature is raised to 120°C, and 660.0g (6.05mol) of 2-aminophenol and 544.9g (9.07mol) of urea It is continuously fed into the horizontal double-helix reactor in proportion, the average residence time of the molten material in the reactor is 0.8h, and the ammonia gas generated is removed from the system in time. The reaction material was transferred to 1320.0g of 70°C water while it was hot, and after continuing to stir for 30min, cooled to 10°C, filtered and dried to obtain 804.9g of benzoxazolone with a content of 98.9% (external standard of liquid chromatography), yield It is 98.5% (based on 2-aminophenol).

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Abstract

The invention relates to the technical field of organic synthesis, in particular to a method for continuously synthesizing benzoxazolinone in a horizontal double-helix reactor at a molten state. Compared with the traditional solvent-free method, the reaction device is the horizontal double-helix reactor, so that the method has the advantages that the operation is simple; heating is uniform; stirring effect is good; reaction time is short; product atom utilization rate is high; the yield is 97.3%-98.5% (based on 2-aminophenol), the content is 98.3%-99.1% (liquid chromatography and external standard), the amount of three wastes is small, treatment is easy, operation is simple, and is convenient for automatic production.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a continuous method for synthesizing benzoxazolone in a solvent-free system. Background technique [0002] Benzoxazolinone is a light yellow solid with a melting point of 140-142°C. Its molecular formula: C 7 h 5 NO 2 , molecular weight: 135.12, molecular structure formula: [0003] [0004] The chemical properties of benzoxazolone are relatively active. For example, the hydrogen atom at the 3-position in its molecular structure can undergo hydroxymethylation reaction with formaldehyde, the hydrogen at the 6-position of the benzene ring is easily replaced by chlorine, and it is easy to open the ring in a strong alkaline medium. Generate 2-hydroxyphenyl amino acid and so on. These properties make benzoxazolone have important applications in pesticide, medicine and other fields. In terms of pesticides, benzoxazolone is an important intermediate of high-efficiency...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D263/58
CPCC07D263/58
Inventor 刘林波田轮胡志彬王宇龚小丽
Owner 湖南速博生物技术有限公司