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Process for preparing 2-fluoro-6-chlorophenyl nitrile

A technology for chlorobenzonitrile and chlorotoluene is applied in the field of preparation of 2-fluoro-6-chlorobenzonitrile, can solve problems such as being unsuitable for large-scale production, difficult to source raw materials, difficult to separate products, etc. Friendly, simple craftsmanship

Inactive Publication Date: 2004-01-07
WUHAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first two methods have the problem of difficult sources of raw materials, and the third method is actually uncontrollable and has disadvantages such as difficult product separation.
Therefore, they are not suitable for large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Will 7.6930 g H 2 C 2 o 4 2H 2 O was dissolved in 30 mL of distilled water at 85°C, and then 4.7060 grams of 85% concentrated phosphoric acid and 3.7010 grams of V 2 o 5 After forming a uniform solution, pour the solution quickly into 30 grams of silica gel (φ125-425 μm). Stir evenly, and after drying, gradually raise the temperature to 580°C in a muffle furnace and keep the temperature for 12 hours. After natural cooling, set aside. The composition of the catalyst is: V 1 P 1 o 4.8 / SiO 2 , The active component weight content of the catalyst is 10%.

[0015] 15g of the above-mentioned solid catalyst is packed in a quartz tube fixed-bed reactor with an internal diameter of 25mm, and the molar ratio of the reaction raw materials is 2-fluoro-6-chlorotoluene:NH 3 :Air=1:7:30, the reaction temperature is 673±1K, and the catalyst load is 50g / (kgcat·h). After reacting under normal pressure for 8 hours, the conversion rate of 2-fluoro-6-chlorotoluene was 99.3%, and...

Embodiment 2

[0017] 11.0103 g H 2 C 2 o 4 2H 2 O was dissolved in 30 mL of distilled water at 85°C, and then 3.3554 grams of 85% concentrated phosphoric acid and 2.6448 grams of V 2 o 5 , after forming a dark blue solution, add 1.4556 g of CrO 3 , 1.0030ml 2.92mol / lTiCl 4solution and 0.3600 g H 3 BO 3 After forming a uniform solution, quickly pour the solution into 30 grams of silica gel (φ125-425 μm). Stir well and let stand overnight. Gradually raise the temperature to 580° C. in a high-temperature furnace and keep the temperature for 12 hours. After cooling naturally, save for later use. The catalyst is composed of: V 1 P 1 Cr 0.5 B 0.2 Ti 0.1 o 6.25 / SiO 2 , The active component weight content of the catalyst is 10%.

[0018] 15g of catalyst is loaded into a fixed-bed reactor with a quartz tube with an inner diameter of 25mm, and the mixed gas of raw materials passes through the catalyst bed for reaction. The molar composition of the raw gas mixture is: 2-fluoro-6-ch...

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Abstract

A process for preparing 2-fluoro-6-chlorophenylnitrile features the reaction of 2-fluoro-6-chlorotoluene as raw material on air and amonia at 632-723 deg.K under the existance of catalyst system. The said catalyst system is composed of primary catalyst (V or P) and cocatalyst (Ti-Fe-Ni-Co or Bi, Mn-Cr-Mo-Cu-Zn or Sn, or B-Na-K-Li or Mg). Its advantages are high output rate (71.47 mol%), and high purity (more than 99%).

Description

technical field [0001] The invention relates to a preparation method of 2-fluoro-6-chlorobenzonitrile, which belongs to the technical field of organic chemistry and also belongs to the technical field of organic fine chemicals. Background technique [0002] 2-fluoro-6-chlorobenzonitrile (2-chloro-6-fluorobenzonitrile), molecular formula ClC 6 h 3 FCN, pure product is white crystal. [0003] One of the best methods for preparing fluorobenzoic acid and fluorobenzamide is to prepare the corresponding fluoroaromatic nitriles from chloroaromatic nitriles through high-temperature fluorination, followed by hydrolysis and reduction reactions. At present, new pesticides and medicines containing fluorine are constantly emerging, and the demand for fluorobenzoic acid and fluorobenzamide has increased sharply. Starting from 2-fluoro-6-chlorobenzonitrile, many compounds in the fields of medicine, pesticides, and photoelectric recording materials can be synthesized. [0004] Before th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/24C07C255/50
Inventor 郑穹李晓芸喻鹏黄驰谢光勇杨元庆贺旭峰
Owner WUHAN UNIV