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High-efficiency synthesis method of 2-cyanophenol

A technology of o-hydroxybenzonitrile and o-hydroxybenzamide, which is applied in the field of organic synthesis, can solve problems such as o-hydroxybenzonitrile that have not yet been seen, achieve continuous production methods, improve safety and environmental protection, and improve conversion rate effect

Inactive Publication Date: 2019-07-23
CHANGZHOU VOCATIONAL INST OF ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] So far, there has been no research on the method of reacting o-hydroxybenzamide solution and phosgene to synthesize o-hydroxybenzonitrile in a microchannel continuous flow mode

Method used

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  • High-efficiency synthesis method of 2-cyanophenol
  • High-efficiency synthesis method of 2-cyanophenol
  • High-efficiency synthesis method of 2-cyanophenol

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Adopt the method for synthesizing o-hydroxybenzonitrile with microchannel reactor of the present invention, take o-hydroxybenzamide and phosgene as reactant raw material to synthesize o-hydroxybenzonitrile, comprise the steps:

[0028] S1: Pretreatment of reactants, dissolving 50 g (0.36 mol) of o-hydroxybenzamide in toluene to prepare 167 g of o-hydroxybenzamide solution with a mass concentration of 30%;

[0029] S2: The setting of the reaction conditions of the microchannel reactor, the heat exchange sheet integrated with the reaction sheet in the microchannel reactor is connected to the external heating and cooling circulator, and the heat exchange medium in the heat exchange sheet is heat transfer oil, through The heating and cooling circulator sets the reaction temperature of the microchannel reactor;

[0030] S3: Synthesis of o-hydroxybenzonitrile, using o-hydroxybenzamide solution with a mass concentration of 30% and phosgene with a purity of 98% as raw materials...

Embodiment 2

[0033] Adopt the method for synthesizing o-hydroxybenzonitrile with microchannel reactor of the present invention, take o-hydroxybenzamide and phosgene as reactant raw material to synthesize o-hydroxybenzonitrile, comprise the steps:

[0034] S1: Pretreatment of reactants, dissolving 50 g (0.36 mol) of o-hydroxybenzamide in xylene to prepare 250 g of o-hydroxybenzamide solution with a mass concentration of 20%;

[0035]S2: The setting of the reaction conditions of the microchannel reactor, the heat exchange sheet integrated with the reaction sheet in the microchannel reactor is connected to the external heating and cooling circulator, and the heat exchange medium in the heat exchange sheet is heat transfer oil, through The heating and cooling circulator sets the reaction temperature of the microchannel reactor;

[0036] S3: Synthesis of o-hydroxybenzonitrile, using o-hydroxybenzamide solution with a mass concentration of 40% and phosgene with a purity of 95% as raw materials, ...

Embodiment 3

[0039] The method for synthesizing o-hydroxybenzonitrile using a microchannel reactor of the present invention uses o-hydroxybenzamide and diphosgene as reactant raw materials to synthesize o-hydroxybenzonitrile, comprising the following steps:

[0040] S1: Pretreatment of reactants, dissolving 50 g (0.36 mol) of o-hydroxybenzamide in xylene to form 500 g of o-hydroxybenzamide solution with a mass concentration of 10%;

[0041] S2: The setting of the reaction conditions of the microchannel reactor, the heat exchange sheet integrated with the reaction sheet in the microchannel reactor is connected to the external heating and cooling circulator, and the heat exchange medium in the heat exchange sheet is heat transfer oil, through The heating and cooling circulator sets the reaction temperature of the microchannel reactor;

[0042] S3: Synthesis of o-hydroxybenzonitrile, using o-hydroxybenzamide solution with a mass concentration of 10% and diphosgene with a purity of 98% as raw ...

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Abstract

The invention discloses a high-efficiency synthesis method of 2-cyanophenol. The high-efficiency synthesis method comprises the four working procedures of pre-processing of reaction substances, setting of reaction conditions of a microchannel reactor, and synthesis and post-processing of 2-cyanophenol. The method synthesizes the 2-cyanophenol product in a means of continuous flow in the microchannel reactor. Compared with an existing technology for synthesizing 2-cyanophenol, the method has the characteristics of precisely controllable reaction conditions, continuous production means, high safety and short reaction time. Meanwhile, the conversion rate of 2-cyanophenol reaction raw materials is as high as 100%, the reaction by-products are less, the quality is high, the product content ishigher than or equal to 98 (liquid chromatography, external standard method), and the yield of 2-cyanophenol product is 90-95% (on the basis of 2-cyanophenol).

Description

technical field [0001] The invention belongs to the technical field of organic synthesis application, and specifically relates to the reaction synthesis of o-hydroxybenzonitrile products in a microchannel reactor using o-hydroxybenzamide solution and phosgene as raw materials. More specifically, it is a process for synthesizing o-hydroxybenzonitrile by using o-hydroxybenzamide solution and phosgene in a Haomai microchannel reactor. Background technique [0002] O-hydroxybenzonitrile (also known as salicylonitrile) is an important fine chemical intermediate. On the one hand, p-hydroxybenzonitrile can be used to produce medical drugs. Body blocking drugs, which are mainly used for the treatment of arrhythmias such as atrial fibrillation and supraventricular tachycardia, angina pectoris and hypertension; ", "Bromoxynil", "Hydroxynil", "Cheltonil" and other benzocyano-based pesticides; at the same time, p-hydroxybenzonitrile can also be used in the field of liquid crystal mater...

Claims

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Application Information

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IPC IPC(8): C07C255/53C07C253/20
CPCC07C253/20C07C255/53
Inventor 乔奇伟王晓东李艳秋赵昊昱李英利蒋涛李树白薛叙明
Owner CHANGZHOU VOCATIONAL INST OF ENG
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