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Method for efficient synthesis of 2-chloro-4-fluoro-5-nitrotrichlorotoluene

A technology of nitrobenzotrichloride and fluorobenzotrichloride, which is applied in the field of efficient synthesis of 2-chloro-4-fluoro-5-nitrobenzotrichloride, can solve problems such as high cost and incomplete nitration reaction, and achieve Effects of increasing mass fraction, enhancing nitrification ability, and enhancing digestion ability

Inactive Publication Date: 2019-01-25
宿州学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of this invention is to provide a method for efficiently synthesizing 2-chloro-4-fluoro-5-nitrobenzotrichloride to solve the problem of incomplete nitration reaction and high cost in the prior art

Method used

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  • Method for efficient synthesis of 2-chloro-4-fluoro-5-nitrotrichlorotoluene
  • Method for efficient synthesis of 2-chloro-4-fluoro-5-nitrotrichlorotoluene
  • Method for efficient synthesis of 2-chloro-4-fluoro-5-nitrotrichlorotoluene

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Experimental program
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Effect test

Embodiment 1

[0024] Get 25.0g (0.10mol) 2-chloro-4-fluorobenzotrichlorotoluene liquid and place in 50mL dropping funnel, the concentrated sulfuric acid that 26.0g mass concentration is 98% and the concentrated nitric acid that 26.0g mass concentration is 98% forms Pour the mixed acid into a 100mL four-necked flask. Under the condition of stirring, open the dropper to slowly add the 2-chloro-4-fluorobenzotrichlorotoluene liquid into the four-necked flask. The dropping time is 1.5h, and the reaction temperature is 0°C. After the dropwise addition, keep warm for 10 minutes, then put the nitrating material into 250g (13.89mol) of ice-water mixture, filter with circulating water vacuum pump, wash and dry to obtain egg yellow 2-chloro-4-fluoro-5-nitrotri Chlorotoluene solid 28.77g, the filtrate and washing water that are sucked out are reclaimed, to recycle. The product yield calculated by weighing is 98.23%, and the product purity is 92.50%.

Embodiment 2

[0026] Get 25.0g (0.10mol) 2-chloro-4-fluorobenzotrichlorotoluene liquid and place in 50mL dropping funnel, the concentrated sulfuric acid that 26.0g mass concentration is 98% and the concentrated nitric acid that 26.0g mass concentration is 98% forms Pour the mixed acid into a 100mL four-necked flask, and under the condition of stirring, open the dropper to slowly add the 2-chloro-4-fluorobenzotrichlorotoluene liquid into the four-necked flask, the dropping time is 1.5h, and the reaction temperature is -2°C , keep warm for 10min after the dropwise addition, then put the nitrating material into 200g (11.12mol) ice-water mixture, carry out suction filtration with a circulating water vacuum pump, wash, and dry to obtain egg yellow 2-chloro-4-fluoro-5-nitro Trichlorotoluene solid 28.70g, the filtrate and washing water that are sucked out are reclaimed, to recycle. The product yield calculated by weighing is 98.01%, and the product purity is 92.32%.

Embodiment 3

[0028] Get 25.0g (0.1mol) of 2-chloro-4-fluorobenzotrichlorotoluene liquid and place it in a 50mL dropping funnel, and use 26.0g mass concentration of 98% concentrated sulfuric acid and 26.0g mass concentration of 98% concentrated nitric acid to form Pour the mixed acid into a 100mL four-necked flask. Under the condition of stirring, open the dropper to slowly add the 2-chloro-4-fluorobenzotrichloride liquid into the four-necked flask. The dropping time is 1.5h, and the reaction temperature is 2°C. After the dropwise addition, keep warm for 10 minutes, then put the nitrating material into 200g (11.12mol) of ice-water mixture, filter with circulating water vacuum pump, wash and dry to obtain egg yellow 2-chloro-4-fluoro-5-nitro Trichlorotoluene solid 29.00g, the filtrate and washing water filtered out by suction are recovered for recycling. The product yield calculated by weighing is 98.17%, and the product purity is 91.98%.

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Abstract

The invention discloses a method for efficient synthesis of 2-chloro-4-fluoro-5-nitrotrichlorotoluene. The method comprises the following steps of (1) a nitrification reaction, wherein concentration sulfuric acid with the mass concentration of 98% and concentrated nitric acid with the mass concentration of 98 % are mixed according to the mass ratio of 1:1 to prepare mixed acid, and 2-chloro-4-fluorotrichlorotoluene is added dropwise into the mixed acid under the condition of stirring to carry out the nitration reaction; (2) quenching of the reaction, wherein a nitrified material obtained afterthe nitrification reaction is put into an ice-water mixture for stirring to quench the reaction; (3) preparation of a dry product, wherein after the reaction is quenched, a circulating water vacuum pump is adopted for suction filtration, and then washing and drying are conducted to obtain the dry product of 2-chloro-4-fluoro-5-nitrotrichlorotoluene; (4) recycling, wherein a filtrate obtained after the suction filtration and washing water are recovered for recycling. The method can improve the production efficiency, the color of the finished product is pure, and the yield and purity of the product are also high and are both 90% or above.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a high-efficiency synthesis method of 2-chloro-4-fluoro-5-nitrobenzotrichloride. Background technique [0002] 2-Chloro-4-fluoro-5-nitrobenzotrichloride is an important fine chemical intermediate and can be used as a starting material for the synthesis of 2-chloro-4-fluoro-5-nitrobenzoic acid and its derivatives. High use value. [0003] The current patents related to the synthesis of 2-chloro-4-fluoro-5-nitrobenzotrichloride or similar products include: a method for preparing benzoic acid derivatives through a new synthetic intermediate (CN 101142168B), and a method for preparing trifluorotoluene derivatives (CN10101891624B), the post-treatment new process of 5-bromo-2-chlorobenzoic acid (CN 107162894B), a kind of synthetic method (CN 106905161A) of 2-chloro-4-fluoro-5-nitrobenzoic acid and 2-chloro - The preparation method of 4-fluoro-5-nitrobenzenesulfo...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C205/12
CPCC07C201/08C07C205/12
Inventor 卞振涛赵旋旋曹红霞郭攀刘程成朱岩岩
Owner 宿州学院
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