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Synthesis method of 3-cyanobenzaldehyde

A synthesis method and technology of cyanobenzene, which is applied in the field of synthesis of 3-cyanobenzaldehyde, can solve the problems of long and complex process route and low yield, and achieve high purity, low equipment requirements and high yield Effect

Inactive Publication Date: 2019-12-03
武穴市阳泰化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the production methods of 3-cyanobenzaldehyde include diazonium salt method, gas-phase catalytic oxidation method, amide dehydration method, etc., but there are obvious shortcomings such as high toxicity, long and complicated process route, high industrial application cost and low yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] A kind of synthetic method of 3-cyanobenzaldehyde of present embodiment, comprises the following steps:

[0014] (1) Take 20mL of 1,3-dimethylbenzene and place it in the reactor, heat the reactor to 132°C, add the solvent N, N-dimethylformamide DMF, catalyst and cocatalyst in sequence, the N, N -The addition amount of dimethylformamide DMF is 22mL, the addition amount of catalyst and co-catalyst is 2.5g and 12.5g respectively, the oxygen feed rate is controlled to be 900mL / min, the hydrogen feed rate is 100mL / min, and the reaction is 4h;

[0015] (2) Cool the above reaction solution to room temperature, and the obtained transparent colorless crystal is 3-methylbenzonitrile. After washing the obtained crystal twice with DMF, remove the DMF solvent by suction filtration to obtain a product with a purity higher than 90 % of 3-methylbenzonitrile;

[0016] (3) Put the 3-methylbenzonitrile synthesized in the above step (2) in the reactor, heat the reactor to 113°C, add the s...

Embodiment 2

[0019] A kind of synthetic method of 3-cyanobenzaldehyde of present embodiment, comprises the following steps:

[0020] (1) Take 20mL of 1,3-dimethylbenzene and put it in the reactor, heat the reactor to 130-135°C, add the solvent N,N-dimethylformamide DMF, catalyst and co-catalyst in sequence, the The add-on of N, N-dimethylformamide DMF is 20mL, the add-on of catalyzer and cocatalyst are respectively 2.8g and 10g, and the control oxygen feed rate is 900mL / min, and the hydrogen feed rate is 100mL / min, the reaction 5h;

[0021] (2) Cool the above reaction solution to room temperature, and the obtained transparent colorless crystal is 3-methylbenzonitrile. After washing the obtained crystal 3 times with DMF, the DMF solvent is removed by suction filtration to obtain a product with a purity higher than 90 % of 3-methylbenzonitrile;

[0022] (3) Put the 3-methylbenzonitrile synthesized in the above step (2) in the reactor, heat the reactor to 110°C, add the solvent N,N-dimethyl...

Embodiment 3

[0024] A kind of synthetic method of 3-cyanobenzaldehyde of present embodiment, comprises the following steps:

[0025] (1) Take 20mL of 1,3-dimethylbenzene and place it in the reactor, heat the reactor to 135°C, add the solvent N,N-dimethylformamide DMF, catalyst and co-catalyst in sequence, the N,N - The addition amount of dimethylformamide DMF is 25mL, the addition amount of catalyst and co-catalyst is 3.0g and 15g respectively, the oxygen feed rate is controlled to be 900mL / min, the hydrogen feed rate is 100mL / min, and the reaction is 5h;

[0026] (2) Cool the above reaction solution to room temperature, and the obtained transparent colorless crystal is 3-methylbenzonitrile. After washing the obtained crystal 3 times with DMF, the DMF solvent is removed by suction filtration to obtain a product with a purity higher than 90 % of 3-methylbenzonitrile;

[0027] (3) Put the 3-methylbenzonitrile synthesized in the above step (2) in the reactor, heat the reactor to 115°C, add t...

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Abstract

The invention discloses a synthetic method of 3-cyanobenzaldehyde. The method comprises the following steps: (1) placing 20mL of 1,3-xylene into a reaction kettle, heating the reaction kettle to 130 to 135 DEG C; sequentially adding dimethyl formamide (DMF), a catalyst and a cocatalyst; (2) cooling the reaction liquid to room temperature to obtain a transparent colorless crystal, namely, 3-methylbenzonitrile; and (3) putting the 3-methylbenzonitrile into a reaction kettle, carrying out heating to 110-115 DEG C, adding DMF, a catalyst and a cocatalyst, controlling the oxygen introduction amountto be 900 mL / min and the hydrogen introduction amount to be 100 mL / min, and carrying out reacting for 2-3 hours to obtain white crystalline powder. According to the invention, the 3-methylbenzonitrile is synthesized from 1,3-xylene through a liquid phase ammoxidation one-step method under normal pressure, and 3-cyanobenzaldehyde is further synthesized through oxidation of 3-methylbenzonitrile, sothat the yield is high, product purity is high, and requirements on the equipment are low.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing 3-cyanobenzaldehyde. Background technique [0002] 3-Cyanobenzaldehyde, the molecular formula is C 8 h 5 NO, the molecular weight is 131.1314, with white crystalline powder, used as a pharmaceutical intermediate. [0003] 3-Cyanobenzaldehyde is mainly used as a pharmaceutical intermediate with important uses and great economic value. At present, the production methods of 3-cyanobenzaldehyde include diazonium salt method, gas-phase catalytic oxidation method, amide dehydration method, etc., but there are obvious shortcomings such as high toxicity, long and complicated process route, high industrial application cost and low yield. . [0004] Therefore, for the many problems that above-mentioned synthetic method exists, the synthetic method of researching and developing a kind of 3-cyanobenzaldehyde is very urgent requirement of this industry....

Claims

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Application Information

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IPC IPC(8): C07C253/30C07C255/56
CPCC07C253/28C07C253/30C07C255/56C07C255/50
Inventor 吴水保
Owner 武穴市阳泰化工股份有限公司
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