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 synthetic method of p-hydroxybenzonitrile. The synthetic method of the p-hydroxybenzonitrile is characterized by comprising the following steps of: dissolving p-hydroxybenzaldehyde and hydroxylamine hydrochloride into an organic solvent; adding a tungsten catalyst; controlling reaction temperature at 80-140 DEG C and reaction time for 8-12 hours; synthesizing the p-hydroxybenzonitrile by one step through the catalysis of the tungsten catalyst. According to the synthetic method disclosed by the invention, the problems of safety of environments, personnel and the like, which are caused by using cyanides, can be fundamentally solved; and besides, the synthetic method disclosed by the invention has the advantages of moderate reaction condition and simple steps and can more meet the requirements of industrial production from the aspects of society, environment, economy, and the like.

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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