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Method used for preparing 3-chlorobenzonitrile

A technology of m-chlorobenzonitrile and chlorobenzonitrile, which is applied in the field of preparation of m-chlorobenzonitrile, can solve the problems of high catalyst and equipment requirements, high reaction temperature, and high operation requirements, and achieve stable quality, continuous reaction process, and simple process Effect

Inactive Publication Date: 2019-11-01
三门峡环宇生化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When using m-chlorotoluene to prepare m-chlorobenzonitrile through ammoxidation, side reactions such as deep oxidation may occur, and the requirements for catalysts and equipment are high, the investment is large, the reaction temperature is high (300-500 ° C), and the operation requirements are high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] First, add 3000g of m-chlorobenzoic acid with a content of 98.0% to a 10L ultrasonic high-pressure thermostat equipped with a thermometer probe, an ultrasonic generator probe, an ammonia pipe and a distillation column, and turn on the heating power supply to raise the temperature. When the temperature rises to 165°C After melting, turn on the stirring, then open the ammonia gas valve and the pressure reducing valve of the liquefied ammonia steel cylinder to pass ammonia to the ultrasonic high-pressure thermostat, the early stage reaction is controlled at 160 ~ 180 ℃, and reacts for 2 h to generate the first ammonium m-chlorobenzoate. In the middle of the reaction mixture, the ammonia flow was stopped. The molar ratio of m-chlorobenzoic acid to ammonia is 1:1.2. The content of ammonium chlorobenzoate in the first intermediate reaction mixture detected by high performance liquid chromatography is 97.3%. During the reaction process, the unreacted and escaped ammonia gas i...

Embodiment 2

[0025] First, add 3000g of m-chlorobenzoic acid with a content of 98.0% to a 10L ultrasonic high-pressure thermostat equipped with a thermometer probe, an ultrasonic generator probe, an ammonia pipe and a distillation column, and turn on the heating power supply to raise the temperature. When the temperature rises to 165°C After melting, turn on the stirring, then open the ammonia gas valve and pressure reducing valve of the liquefied ammonia steel cylinder to feed ammonia to the ultrasonic high-pressure thermostat, the reaction temperature in the early stage is controlled at 160~180°C, and react for 2h to generate the first ammonium m-chlorobenzoate In the middle of the reaction mixture, the ammonia flow was stopped. The molar ratio of m-chlorobenzoic acid to ammonia is 1:1.2. The content of ammonium m-chlorobenzoate in the first intermediate reaction mixture detected by high performance liquid chromatography was 97.3%. The ammonia gas escaped during the reaction is absorbed...

Embodiment 3

[0029]First, add 300g of m-chlorobenzoic acid with a content of 98.0% to a 1L microwave constant temperature autoclave equipped with a thermometer and a distillation column, turn on the heating power supply to raise the temperature, when the temperature rises to 165°C and basically melts, turn on the stirring, and then turn on the liquid ammonia The ammonia gas valve of steel cylinder and pressure reducing valve lead ammonia to microwave constant temperature autoclave, and early stage reaction is controlled at 160~180 ℃, reacts 2h, generates the first intermediate reaction mixture containing ammonium m-chlorobenzoate, stops flowing ammonia. The molar ratio of m-chlorobenzoic acid to ammonia is 1:1.2. The content of ammonium chlorobenzoate in the first intermediate 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.

[0030] Then slowly he...

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Abstract

The invention provides a method used for preparing 3-chlorobenzonitrile, and belongs to the technical field of organic chemistry, and organic fine chemical technology. The method comprises following steps: 3-chlorobenzoic acid is reacted with ammonia to generate a first intermediate reaction mixture containing 3-chlorobenzoic acid ammonium; the first intermediate reaction mixture containing 3-chlorobenzoic acid ammonium is subjected to dehydration reaction to obtain a second intermediate reaction mixture containing 3-chlorobenzamide; the second intermediate reaction mixture containing 3-chlorobenzamide is subjected to dehydration reaction to obtain a mixture containing 3-chlorobenzonitrile; and the mixture containing 3-chlorobenzonitrile is subjected to physical processing to obtain finished product 3-chlorobenzonitrile. The route is short; operation is simple; reaction conditions are simple and are convenient to control; production cost is low; environment is low; the quality of synthesized 3-chlorobenzonitrile is stable; in the 3-chlorobenzoic acid and ammonia reaction system, supersonic wave or microwave catalytic dehydration is adopted in a middle later period, and 3-chlorobenzonitrile yield and purity are increased obviously.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and also belongs to the technical field of organic fine chemicals, and specifically relates to a preparation method of m-chlorobenzonitrile. Background technique [0002] M-chlorobenzonitrile, also known as m-chlorobenzonitrile and 3-chlorobenzonitrile, is an important fine chemical and an intermediate in organic preparation. Due to the chemical activity of the aromatic cyano group of m-chlorobenzonitrile, a series of fine chemical products can be synthesized through hydrolysis, hydrogenation, addition or polycondensation reactions, which are important for the manufacture of pesticides, medicines, dyes, spices, resins, etc. Raw materials, for example, can be used to synthesize m-chlorobenzylamine and bupropion. [0003] At present, there are mainly two kinds of preparation methods of m-chlorobenzonitrile. One method is to synthesize m-chlorobenzaldehyde oxime with m-chlorobenzaldehyde ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/20C07C255/50
CPCC07C253/20C07C231/02C07C255/50C07C233/65
Inventor 段敬杰张卫民梁振贤魏战勇谭静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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