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Synthetic method of dichlorobenzonitrile

A technology for the synthesis of p-fluorobenzonitrile, which is applied in the direction of nitrogen oxide-organic compound reaction preparation, chemical recovery, organic chemistry, etc., can solve the problems of high temperature requirements, increased energy consumption, etc., and achieve mild reaction conditions , the effect of simple steps

Inactive Publication Date: 2012-03-28
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above-mentioned first method has relatively high temperature requirements, which will increase energy consumption in industrial production, and may produce highly corrosive hydrofluoric acid in the production process, which has higher requirements on equipment.

Method used

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  • Synthetic method of dichlorobenzonitrile
  • Synthetic method of dichlorobenzonitrile
  • Synthetic method of dichlorobenzonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: the preparation of phosphotungstic acid tetramethylammonium salt catalyst (catalyst A)

[0031] h 3 PW 12 o 40 +3(CH 3 ) 4 NOH→[(CH 3 ) 4 N] 3 [P(W 3 o 10 ) 4 ]

[0032] Tetramethylammonium hydroxide (25% aqueous solution) 1.5g, phosphotungstic acid 3.9g, add 20ml water and stir for 3h, then add 2.8g silicon oxide and stir for 24h, evaporate the solvent to obtain the desired catalyst; wherein phosphotungstate and The mass ratio of silicon oxide is 1.5:1.

Embodiment 2

[0033] Embodiment 2: the preparation of silicotungstic acid tetraethylammonium salt catalyst (catalyst B)

[0034] h 4 SiW 12 o 40 +4(C 2 h 5 ) 4 NOH→[(C 2 h 5 ) 4 N] 4 [Si(W 3 o 10 ) 4 ]

[0035] Tetraethylammonium hydroxide (25% aqueous solution) 3.8g, silicotungstic acid 4.8g, add 20ml water and stir for 3h, then add 2.8g silicon oxide and stir for 24h, evaporate the solvent to obtain the required catalyst; wherein silicotungstate and The mass ratio of silicon oxide is 2:1.

Embodiment 3

[0036] Embodiment 3: the preparation of phosphomolybdic acid tetramethylammonium salt catalyst (catalyst C)

[0037] h 3 PMo 12 o 40 +3(CH 3 ) 4 NOH→[(CH 3 ) 4 N] 3 [P(Mo 3 o 10 ) 4 ]

[0038] Tetrabutylammonium hydroxide (40% solution) 6.2g, phosphomolybdic acid 6g, add 20ml water and stir for 3h, then add 2.8g silicon oxide and stir for 24h, evaporate the solvent to obtain the desired catalyst; wherein the mass of phosphomolybdate and silicon oxide The ratio is 3:1.

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Abstract

The invention relates to a synthetic method of dichlorobenzonitrile, which is characterized in that dichlorobenzonitrile and oxammonium hydrochloride are resolved in an organic solvent, and the dichlorobenzonitrile is catalyzed and synthesized through a heteropoly salt catalyst, the reaction temperature is controlled to range from 80 to130 DEG C, and the reaction lasts for 8 to 12h. In the invention, cyanide is not used as raw materials, the method is simple and feasible, the product yield is high, the process flow is simple, the requirements of equipment are low, and the catalyst can be recovered for reutilization.

Description

technical field [0001] The invention relates to a synthesis method of p-fluorobenzonitrile, in particular to a method for synthesizing p-fluorobenzonitrile by catalyzing p-fluorobenzaldehyde and hydroxylamine hydrochloride through a heteropolyacid salt catalyst. Background technique [0002] p-Fluorobenzonitrile is an important intermediate for the synthesis of various pesticides, dyes and medicines. In terms of pesticides, synthesize a variety of pyridine or pyrimidine derivative herbicides; in medicine, synthesize pyridoimidazolone derivatives for the treatment of oxidative unsaturated fatty acid diseases, synthesize inhibitory cytokinin anti-inflammatory drugs, anticoagulant Blood agents, elastase inhibitors, antidiuretic hormone antagonists and oxytocin antagonists, etc. Moreover, this compound can also be used to prepare optical materials such as liquid crystals. Because p-fluorobenzonitrile is widely used, it is of great significance to develop this intermediate. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/50C07C253/02
CPCY02P20/584
Inventor 黄军裴为格黄磊
Owner NANJING UNIV OF TECH
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