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Synthesis method of trifluralin

A synthetic method, trifluralin technology, applied in chemical instruments and methods, amino compound preparation, organic compound preparation, etc., can solve the problems of long synthesis time, environmental hazards, high energy consumption, etc., and achieve low equipment requirements and three wastes The effect of low emission and high conversion rate of raw materials

Active Publication Date: 2020-02-07
YANCHENG TEACHERS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method takes a long time to synthesize, consumes a lot of energy, and produces a large amount of three wastes in production, which is harmful to the environment.

Method used

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  • Synthesis method of trifluralin
  • Synthesis method of trifluralin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 250ml reactor, add 4-chloro-3,5-dinitrobenzotrifluoride (27.06g, 0.1mol), vitamin C (0.135g), and 30mL water in sequence, and di-n-propylamine (12.14 g, 0.12mol), sodium hydroxide solution (4g of sodium hydroxide dissolved in 16mL of water), the dropwise addition was completed within 30 minutes, and the pH of the system was adjusted to 7.5 to 8.5 with a 1% aqueous sodium hydroxide solution by mass percentage, and the pH of the system was adjusted at 60°C After 2.0 hours of reaction, crystals were precipitated after cooling to room temperature, filtered, washed with water until neutral, and dried to obtain 33.02 g of the target compound with a yield of 98.5% (based on 4-chloro-3,5-dinitrotrifluorotoluene). The product has a purity of 99 wt%, and a nitrosamine content of 0.6 ppm.

Embodiment 2

[0028] In a 250ml reactor, add 4-chloro-3,5-dinitrobenzotrifluoride (27.06g, 0.1mol), vitamin C (0.27g), and 30mL water successively, and di-n-propylamine (10.12 g, 0.1mol), sodium hydroxide solution (4g of sodium hydroxide dissolved in 16mL of water), the dropwise addition was completed within 30 minutes, and the pH of the system was adjusted to 7.5 to 8.5 with 1% by mass percent sodium hydroxide aqueous solution, and the pH of the system was adjusted at 70°C After 1.5 hours of reaction, crystals were precipitated after cooling to room temperature, filtered, washed with water until neutral, and dried to obtain 33.02 g of the target compound with a yield of 98.5% (calculated as 4-chloro-3,5-dinitrotrifluorotoluene). The product has a purity of 99 wt%, and a nitrosamine content of 0.5 ppm.

Embodiment 3

[0030] In a 250ml reactor, add 4-chloro-3,5-dinitrobenzotrifluoride (27.06g, 0.1mol), vitamin C (0.27g), and 30mL water successively, and di-n-propylamine (10.12 g, 0.1mol), sodium hydroxide solution (4g of sodium hydroxide dissolved in 16mL of water), the dropwise addition was completed within 30 minutes, and the pH of the system was adjusted to 7.5 to 8.5 with a 1% aqueous solution of sodium hydroxide by mass percentage, at 80°C The reaction was carried out for 1.0 hour, and crystals were precipitated after cooling to room temperature, filtered, washed with water until neutral, and dried to obtain 33.05 g of the target compound with a yield of 98.6% (calculated as 4-chloro-3,5-dinitrotrifluorotoluene). The product has a purity of 99% by weight and a nitrosamine content of 0.4ppm.

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Abstract

The invention discloses a synthesis method of trifluralin. The method uses 4-chloro-3,5-dinitrotrifluorotoluene and di-n-propylamine as raw materials, a base as an acid binding agent, and vitamin C asan auxiliary agent, and the target compound is prepared under heating. The advantages of the method are as follows: (1) the used raw materials and auxiliary materials are wide in source, and convenient in preparation; (2) the catalytic effect is good, a raw material conversion rate is high, and the product selectivity is good; and (3) the content of N-nitroso-di-n-propylamine in the product is low, the post-treatment is simple and convenient, the method is a new preparation process of trifluralin, and the large-scale industrial development is facilitated.

Description

[0001] a technical field [0002] The invention relates to a synthesis method of trifluralin, belonging to the technical field of chemical material preparation. This method is suitable for preparing the target by heating reaction under normal pressure with 4-chloro-3,5-dinitrobenzotrifluorotoluene and di-n-propylamine as raw materials, alkali as acid-binding agent, vitamin C as auxiliary agent, and water as reaction medium. In the case of compounds. [0003] Two background technology [0004] Fluoraline (2,6-dinitro-N, N-dipropyl-4-(trifluoromethyl)aniline) Chinese alias: 2,6-dinitro-N, N-dipropyl-4-trifluoromethylaniline, It is orange-yellow crystal, with a melting point of 48.5°C-49°C (original drug 43°C-47.5°C), a boiling point of 139°C-140°C, and a density of 1.36g / cm3 (22°C). Solubility in water at 25°C: 0.184g / L at pH5, 0.221g / L at pH=7, 0.189g / L at pH9; in acetone, chloroform, acetonitrile, toluene, ethyl acetate at 25°C The solubilities are all greater than 1 000g / L,...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/10
CPCC07C209/10C07C211/52
Inventor 方东郑龙洲孙世新李付香毛栋
Owner YANCHENG TEACHERS UNIV
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