Synthetic method for 2-chlorobenzonitrile

A technology of o-chlorobenzonitrile and synthesis method, which is applied in chemical instruments and methods, preparation of organic compounds, purification/separation of carboxylic acid nitrile, etc., can solve the problem of high price of o-chlorobenzaldoxime, influence on yield and product quality, The effect is not very ideal and other problems, to achieve the effect of easy environmental protection treatment, avoiding complicated equipment, and strong market competitiveness

Active Publication Date: 2019-11-08
三门峡环宇生化科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wastewater treatment is difficult and costly
[0019] Some of the above synthetic methods have low conversion rate, some raw materials are expensive and difficult to obtain, high toxicity, serious pollution of three wastes, some reaction process is easy to block, difficult to operate and other defects, the effect is not very ideal
[0020] Among the above-mentioned methods, the first and fourth methods are the simplest (one-step synthesis), but the first raw material o-chlorobenzaldoxime is expensive and difficult to purchase in large quantities, and a large amount of raw material sulfamic acid is produced in the o-chlorobenzoic acid synthesis method. Waste slag affects the yield and product quality, and brings environmental protection treatment problems

Method used

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  • Synthetic method for 2-chlorobenzonitrile
  • Synthetic method for 2-chlorobenzonitrile
  • Synthetic method for 2-chlorobenzonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 200 g of o-chlorobenzoic acid with a content of 98.0% to a 500ml four-necked flask equipped with a thermometer, an ammonia pipe and a distillation column, turn on the power supply of the heating mantle to raise the temperature, and when the temperature rises to 145°C, it basically melts, and then turn on the liquid The ammonia gas valve and the pressure reducing valve of the ammonia steel cylinder pass ammonia, open and stir, and the early stage reaction is controlled at 140~180 ℃, and reacts for 1~2h, taking 2 h as an example, stop passing ammonia. The molar ratio of o-chlorobenzoic acid to ammonia is 1:1.5. The content of ammonium o-chlorobenzoate in the reactant was detected by high performance liquid chromatography to be 97.2%. During the reaction process, the unreacted and escaped ammonia gas is absorbed by water to generate ammonia water.

[0041] Slowly raise the temperature, and react at 230-250° C. for 1-5 hours. Taking the reaction for 1.5 hours as an exa...

Embodiment 2

[0045] Add 200 g of o-chlorobenzoic acid with a content of 98.0% to a 500ml four-necked flask equipped with a thermometer, an ammonia pipe and a distillation column, turn on the power supply of the heating mantle to raise the temperature, and when the temperature rises to 145°C, it basically melts, and then turn on the liquid The ammonia gas valve and the pressure reducing valve of the ammonia steel cylinder are connected to the ammonia, and the stirring is turned on. The initial reaction is controlled at 140-180° C., and the reaction is 1-2 hours. Taking the reaction for 2 hours as an example, the ammonia flow is stopped. The molar ratio of o-chlorobenzoic acid to ammonia is 1:1.5. The content of ammonium o-chlorobenzoate in the reactant was detected by high performance liquid chromatography to be 97.1%. During the reaction process, the unreacted and escaped ammonia gas is absorbed by water to generate ammonia water.

[0046] Slowly raise the temperature, and react at 230~25...

Embodiment 3

[0050] Add 3000g of o-chlorobenzoic acid with a content of 98.0% to a 10L ultrasonic constant temperature kettle equipped with a thermometer probe, an ultrasonic generator probe, an ammonia pipe and a distillation column, turn on the heating power supply, and basically melt when the temperature rises to 145°C , start stirring, then open the ammonia gas valve and the pressure reducing valve of the liquid ammonia steel cylinder to pass through the ammonia, the early stage reaction is controlled at 140~180°C, react for 1~2h, take the reaction 2 h as an example to stop passing through the ammonia. The molar ratio of o-chlorobenzoic acid to ammonia is 1:1.2. The content of ammonium o-chlorobenzoate in the reactant was detected by high performance liquid chromatography to be 97.3%. During the reaction process, the unreacted and escaped ammonia gas is absorbed by water to generate ammonia water.

[0051] Slowly raise the temperature, turn on the ultrasonic generator at the same time...

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Abstract

A synthetic method for 2-chlorobenzonitrile is disclosed and includes the following steps: performing a reaction on o-chlorobenzoic acid and ammonia to generate ammonium o-chlorobenzoate, high temperature dehydration is performed to produce 2-chlorobenzamide, and the high temperature dehydration is performed again to generate the 2-chlorobenzonitrile. In a production process, especially ultrasonicor microwave catalyzed high temperature dehydration is utilized to produce the 2-chlorobenzonitrile, the yield is up to 93%, and the purity of products can reach 97%. And the method has the characteristics of short process route, high reaction yield, good product purity, safe and clean whole reaction process, and easy environmentally friendly treatment. Production of waste water of the 2-chlorobenzonitrile can be effectively reduced, clean production of the 2-chlorobenzonitrile is achieved, unreacted raw material o-chlorobenzoic acid and intermediates can be recovered and then recycled and utilized, and the production cost can be significantly reduced. Moreover, the method can avoid the defects that traditional process equipment is complex, is high in operation requirements and is low inproduct yield, has the characteristics of less "three wastes" and less pollution, is another ideal way to achieve industrial production, and has strong market competitiveness.

Description

technical field [0001] The invention relates to a synthesis method of organic fine chemicals, in particular to a synthesis method of o-chlorobenzonitrile. Background technique [0002] The traditional preparation methods of o-chlorobenzonitrile are generally prepared from corresponding aldehydes and aldoximes as raw materials. These methods have high raw material prices and serious environmental pollution. [0003] O-chlorobenzonitrile (OCBN), also known as o-chlorobenzonitrile and 2-chlorobenzonitrile, is an important fine chemical and an intermediate in organic synthesis. Using o-chlorobenzonitrile as raw material, the corresponding o-chlorobenzylamine, o-chloroaniline, o-fluorobenzonitrile, o-fluorobenzoic acid, o-fluoroaniline, etc. can be prepared, which are widely used in dyestuff, medicine, pesticide and spice industries. It is an important intermediate in the synthesis of new antimalarial drug nitroquine, antihypertensive drug valsartan, uracil herbicides and phenyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/20C07C253/34C07C255/50
CPCC07C253/20C07C231/02C07C253/34C07C255/50C07C233/65Y02P20/584
Inventor 张卫民梁振贤魏战勇谭静段敬杰张坤王馨悦王艳王志全
Owner 三门峡环宇生化科技有限公司
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