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Method for synthesizing salicylonitrile by adopting microchannel reactor

A micro-channel reactor, o-hydroxybenzonitrile technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid nitrile, etc., can solve problems such as unseen o-hydroxybenzonitrile, and achieve continuous production mode Chemical, high quality, improved safety and environmental effects

Inactive Publication Date: 2019-07-12
CHANGZHOU VOCATIONAL INST OF ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] So far, there has been no research on the method for the reaction of o-chlorobenzonitrile and sodium methylate solution to synthesize o-hydroxybenzonitrile in the microchannel continuous flow mode

Method used

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  • Method for synthesizing salicylonitrile by adopting microchannel reactor
  • Method for synthesizing salicylonitrile by adopting microchannel reactor
  • Method for synthesizing salicylonitrile by adopting microchannel reactor

Examples

Experimental program
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Embodiment 1

[0027] The method for synthesizing o-hydroxybenzonitrile using a microchannel reactor of the present invention is to synthesize o-hydroxybenzonitrile with sodium methylate and o-chlorobenzonitrile as reactant raw materials, comprising the following steps:

[0028] S1: Pretreatment of reactants, respectively dissolving 48g (0.88mol) of sodium methoxide and 60g (0.44mol) of o-chlorobenzonitrile in anhydrous methanol to form a sodium methoxide solution with a mass concentration of 40% and a mass concentration of 40% o-chlorobenzonitrile solution;

[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 set the reaction temperature of the microchannel reactor to 110°C, and set the pressure of ...

Embodiment 2

[0033] The method for synthesizing o-hydroxybenzonitrile using a microchannel reactor of the present invention is to synthesize o-hydroxybenzonitrile with sodium methylate and o-chlorobenzonitrile as reactant raw materials, comprising the following steps:

[0034] S1: Pretreatment of reactants, respectively dissolving 120g (2.22mol) of sodium methoxide and 100g (0.73mol) of o-chlorobenzonitrile in anhydrous methanol to form a sodium methoxide solution with a mass concentration of 30% and a mass concentration of 50% o-chlorobenzonitrile solution;

[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 to 140°C, and sets the pressure...

Embodiment 3

[0039] The method for synthesizing o-hydroxybenzonitrile using a microchannel reactor of the present invention is to synthesize o-hydroxybenzonitrile with sodium methylate and o-chlorobenzonitrile as reactant raw materials, comprising the following steps:

[0040] S1: Reactant pretreatment, respectively dissolving 40g (0.74mol) of sodium methoxide and 100g (0.73mol) of o-chlorobenzonitrile in anhydrous methanol to form a sodium methoxide solution with a mass concentration of 5% and a mass concentration of 20% o-chlorobenzonitrile solution;

[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 to 200°C, and sets the pressure of th...

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Abstract

The invention discloses a method for synthesizing salicylonitrile by adopting a microchannel reactor. The method comprises four procedures, i.e., reactant pretreatment, setting of reaction conditionsof the microchannel reactor, synthesis of the salicylonitrile and aftertreatment. According to the method, the salicylonitrile product is synthesized in the microchannel reactor in a continuous flow manner; compared with the existing process for synthesizing the salicylonitrile, the method disclosed by the invention has the characteristics that the reaction conditions are accurate and controllable, the mode of production is continuous, the safety is high, and the reaction time is short; and the conversion ratio of an o-chlorobenzonitrile reactant reaches 100%, reaction byproducts are few, thequality is high, the product content is not lower than 98% (liquid chromatography, external standard method), and the yield of the salicylonitrile product reaches 90% to 95% (by o-chlorobenzonitrile).

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-chlorobenzonitrile solution and sodium methoxide solution as raw materials. More specifically, it is a process for synthesizing o-hydroxybenzonitrile by using o-chlorobenzonitrile and sodium methylate solution 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 ...

Claims

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Application Information

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IPC IPC(8): C07C253/30C07C255/53
CPCC07C253/30
Inventor 王晓东乔奇伟刘承先李英利蒋涛李树白薛叙明李艳秋
Owner CHANGZHOU VOCATIONAL INST OF ENG
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