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Technology of synthesizing 2-hydroxybenzonitrile through one-step method

A technology of hydroxybenzonitrile and step method, which is applied in the field of synthesis of pesticides and pharmaceutical intermediates, can solve the problems of resource waste, increase industrial costs, and produce a large amount of waste liquid, so as to reduce labor intensity, reduce three wastes, and improve production effect of ability

Inactive Publication Date: 2018-11-23
TAIZHOU BAILLY CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although homogeneous catalysis has the characteristics of fast reaction speed and high conversion rate, the separation of products, solvents and catalysts in homogeneous catalysis is complicated, the process is complicated, and the industrial cost is increased; moreover, a large amount of waste liquid will be generated in the production process, resulting in waste of resources. ; At the same time, a large amount of waste liquid pollutes the environment, which does not conform to the principles of green chemistry proposed by the international community.

Method used

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  • Technology of synthesizing 2-hydroxybenzonitrile through one-step method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Put 2.0g (0.0218mol) salicylamide in the vaporizer, 5g 5%wtV 2 o 5 / Al 2 o 3 As for the supported catalyst in the quartz glass tube of the fixed-bed reactor, the vacuum pressure is lower than 50kp by a vacuum pump, and the nitrogen pressure is 0.01MPa to purge for 2 minutes. , the heating ceramic temperature was set to 400°C, and the temperature of the temperature control tube was set to 150°C. After the receiving tank could not receive the product, the reaction was over, and the yield was 75.6% after chromatographic analysis.

Embodiment 2

[0035] Put 2.0g (0.0218mol) salicylamide in the vaporizer, 5g 5%wtV 2 o 5 / Al 2 o 3 As for the supported catalyst in the quartz glass tube of the fixed-bed reactor, the vacuum pressure is lower than 50kp by a vacuum pump, and the ammonia pressure is 0.01MPa to purge for 2 minutes. °C, the temperature of the heating ceramics was set to 400 °C, and the temperature of the temperature control tube was set to 150 °C. After the receiving tank could not receive the product, the reaction was over, and the yield was 85.6% after chromatographic analysis.

Embodiment 3

[0037] Put 2.0g (0.0218mol) salicylamide in the vaporizer, 5g 5%wtV 2 o 5 / Al 2 o 3 As for the supported catalyst in the quartz glass tube of the fixed bed reactor, the vacuum pressure is lower than 50kp through a vacuum pump, and the nitrogen pressure is 0.01MPa to purge for 2min. Then, the temperature of the vaporization furnace was set to 270°C, the temperature of the heating ceramic was set to 380°C, and the temperature of the temperature control tube was set to 150°C. When the receiving tank could not receive the product, the reaction was completed, and the yield was 78.7% after chromatographic analysis.

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Abstract

The invention provides a technology of synthesizing 2-hydroxybenzonitrile through a one-step method. The technology comprises the following steps that 1, a vanadium oxide loaded catalyst is placed into a fixed bed reactor, and by conducting vacuuming through a double-row pipe and sweeping through inert gas, water and air are removed; 2, a certain amount of salicylamide is converted to gas at a certain temperature through a vaporization furnace; 3, the gaseous salicylamide enters the fixed bed reactor, wherein the bed height of the catalyst is 2-3 cm; 4, a product condenses through a temperature control pipe and flows into a receiving tank in a liquid mode. The 2-hydroxybenzonitrile prepared through the method is high in yield, the technology process is simple, the cost is low, and the technology is clean and efficient.

Description

technical field [0001] The invention relates to the field of synthesis of pesticides and pharmaceutical intermediates, in particular to a process for synthesizing 2-hydroxybenzonitrile by one-step method, especially a process for preparing 2-hydroxybenzonitrile by one-step gas-solid phase reaction. Background technique [0002] 2-Hydroxybenzonitrile is an intermediate in the synthesis of pesticides and medicines. It is often used as an intermediate in the organic synthesis of bunilol and the fungicide azoxystrobin. There are several common synthetic methods of 2-hydroxybenzonitrile: [0003] (1) First, salicylaldehyde and hydroxylamine hydrochloride generate salicylaldoxime, and then dehydrate in the dehydrating agent acetic anhydride or thionyl chloride to obtain 2-hydroxybenzonitrile. (2) Salicylamide can obtain 2-hydroxybenzonitrile under the action of dehydrating agent phosgene (or diphosgene, triphosgene, etc.), thionyl chloride, and phosphorus oxychloride. [0004] A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/53C07C253/20B01J23/22B01J23/30
CPCB01J23/002B01J23/22B01J23/30B01J2523/00C07C253/20C07C255/53B01J2523/31B01J2523/55B01J2523/69
Inventor 胡红一汪静莉刘志平郎万中杨露常亚军
Owner TAIZHOU BAILLY CHEM CO LTD
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