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Synthetic method of p-hydroxybenzonitrile

A technology for p-hydroxybenzonitrile and p-hydroxybenzaldehyde is applied in the field of p-hydroxybenzonitrile synthesis, can solve problems such as three wastes and the like, and achieve the effects of simple steps and mild reaction conditions

Inactive Publication Date: 2013-10-30
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, a large amount of formic acid and sodium hydroxide are used in the reaction, the reaction is carried out in two steps, and there are three wastes, so there are no small constraints in terms of economy and operation

Method used

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  • Synthetic method of p-hydroxybenzonitrile
  • Synthetic method of p-hydroxybenzonitrile
  • Synthetic method of p-hydroxybenzonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: the preparation of catalyst 1

[0026] h 3 PW 12 o 40 +3(n-C 4 h 9 ) 4 NOH→[(n-C 4 h 9 ) 4 N] 3 [P(W 3 o 10 ) 4 ]

[0027] Tetrabutylammonium hydroxide (25% methanol solution) 6.2g, phosphotungstic acid 5.8g, add 20ml water and stir for 3h, then add 14.6g silicon oxide and stir for 24h, evaporate the solvent to obtain the required catalyst; The mass ratio of silicon is 1:2.

Embodiment 2

[0028] Embodiment 2: the preparation of catalyst 2

[0029] h 4 SiW 12 o 40 +4(n-C 4 h 9 ) 4 NOH→[(n-C 4 h 9 ) 4 N] 4 [Si(W 3 o 10 ) 4 ]

[0030]Tetrabutylammonium hydroxide (25% methanol solution) 8.3g, silicotungstic acid 5.8g, add 20ml of water and stir for 3h, then add 15.6g of silicon oxide and stir for 24h, evaporate the solvent to get the required catalyst; The mass ratio of silicon is 1:2.

Embodiment 3

[0031] Embodiment 3: the preparation of catalyst 3

[0032] h 3 PW 12 o 40 +3(n-C 4 h 9 ) 4 POH→[(n-C 4 h 9 ) 4 P] 3 [P(W 3 o 10 ) 4 ]

[0033] Tetrabutyl phosphorus hydroxide (40% solution) 4.1g, phosphotungstic acid 5.8g, add 20ml water and stir for 3h, then add 29.2g silicon oxide and stir for 24h, evaporate the solvent to get the required catalyst; wherein phosphotungstate and silicon oxide The mass ratio is 1:4.

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Abstract

The invention relates to a synthesis method of p-hydroxybenzonitrile, which is characterized in that p-hydroxybenzaldehyde and hydroxylamine hydrochloride are dissolved in an organic solvent, a tungsten catalyst is added, the reaction temperature is controlled to 80 to 140°C, and the reaction time is 8 to 12 hours. , one-step synthesis of p-hydroxybenzonitrile via tungsten catalyst catalysis. The synthesis method of the present invention can fundamentally solve the environmental and personnel safety problems caused by the use of cyanide. In addition, the synthesis method of the present invention has mild reaction conditions and simple steps, and is more suitable for the needs of industrial production from social, environmental, economic and other aspects.

Description

technical field [0001] The invention relates to a novel synthesis method of p-hydroxybenzonitrile, in particular to a method for one-step synthesis of p-hydroxybenzonitrile from p-hydroxybenzaldehyde and hydroxylamine hydrochloride via a tungsten catalyst. Background technique [0002] p-Hydroxybenzonitrile is an intermediate of organophosphorus insecticides fenitronil and benzonitrile, an intermediate of herbicide bromoxynil, and an intermediate of liquid crystal materials, spices, etc. There are many ways to synthesize, the early method is T.Sandmeyer method, but the synthesis method has many steps, harsh reaction conditions, using cyanide as raw material, equivalent CuCN as catalyst, easy to cause serious pollution to the environment, and high production cost , these problems have seriously restricted industrial applications, so people try to utilize other approaches to realize the synthesis of p-hydroxybenzonitrile, thereby avoiding the use of this type of highly toxic c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/53C07C253/00
Inventor 黄军陈晓蓉黄磊张瑞
Owner NANJING TECH UNIV
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