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Preparation method of substituted benzyl cyanide

A phenylacetonitrile and reaction technology, applied in the field of organic synthesis, can solve the problems of low reaction efficiency, large floor space, complex equipment and the like, and achieve the effects of simple process route, less equipment and high reaction efficiency

Active Publication Date: 2017-01-25
HEBEI CHENGXIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process mainly adopts kettle-type intermittent production, the reaction efficiency is not high, and many people are employed.
Although CN201110020822.2 adopts the device and method of continuous cyanation reaction, it adopts the series mode of batch kettles to realize continuous operation, the equipment is complicated, and the floor area is large, which is not conducive to operation

Method used

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  • Preparation method of substituted benzyl cyanide
  • Preparation method of substituted benzyl cyanide
  • Preparation method of substituted benzyl cyanide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040]Simultaneously the mol ratio of accurate metering is: benzyl chloride: benzyl chloride and hydrogen cyanide gas that hydrogen cyanide is 1.6: 1.0 are respectively preheated to 155.0 ℃, then enter the microchannel reactor after input mixer mix simultaneously, ensure The molar ratio of the two is always stable at 1.6:1.0, and the nucleophilic substitution reaction is carried out at 180.0°C and 1.5MPa pressure to generate substituted phenylacetonitrile and hydrogen halide. The reaction residence time is 40s, and then the reaction material is cooled to 85°C to quench the reaction. Then introduce the material into the water washing tower to wash off the hydrogen chloride generated by the reaction, let it stand for liquid separation, add 10% sodium bicarbonate solution to the organic phase to neutralize to a pH value of 6.8, let it stand for liquid separation, add water to wash once, and let it stand for further separation. liquid. Then rectify under the pressure of 300Pa to o...

Embodiment 2

[0042] At the same time, the accurately metered molar ratio of o-chlorobenzyl chloride: hydrogen cyanide is 1.8:1.0, and the o-chlorobenzyl chloride and hydrogen cyanide gas are preheated to 165.0°C respectively, and then input into the mixer at the same time to mix and then enter the microchannel Reactor, to ensure that the molar ratio of the two is constantly stable at 1.8:1.0, nucleophilic substitution reaction is carried out at 175.0°C and 1.7MPa pressure to generate o-chlorophenylacetonitrile and hydrogen chloride, the reaction residence time is 90s, and then the reaction material is cooled to 90°C, Quench the reaction, then introduce the material into the water washing tower to wash away the hydrogen chloride generated by the reaction, let it stand for liquid separation, add 5% sodium carbonate solution to the organic phase to neutralize to pH 7.2, let it stand for liquid separation, add water to wash once, and let it stand for liquid separation. Set aside for redistribut...

Embodiment 3

[0044] At the same time, the accurately measured molar ratio is: o-methylbenzyl chloride: hydrogen cyanide 1.8:1.0 o-methylbenzyl chloride and hydrogen cyanide gas were preheated to 175.0 ° C, and then simultaneously input into the mixer and mixed into the Microchannel reactor, to ensure that the molar ratio of the two is always stable at 1.8:1.0, the nucleophilic substitution reaction is carried out at 190.0 ° C and 1.8 MPa pressure to generate o-toluene acetonitrile and hydrogen chloride, the reaction residence time is 120s, and then the reaction material is cooled to 80°C, quench the reaction, then introduce the material into the water washing tower to wash away the hydrogen chloride generated by the reaction, let it stand for liquid separation, add 5% calcium hydroxide solution to the organic phase to neutralize to pH 6.5, let it stand for liquid separation, and then add water Wash once, let stand and then separate liquid. Then rectify under the pressure of 260Pa to obtain...

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Abstract

The invention relates to the technical field of organic synthesis, in particular to a method of continuously preparing a substituted benzyl cyanide compound by using a microchannel reactor, and discloses a preparation method of substituted benzyl cyanide. The preparation method comprises the steps of preheating accurately metered raw materials, namely substituted benzyl halide and hydrogen cyanide gas separately, allowing the raw materials to enter a microchannel reactor after mixing for nucleophilic substitution reaction at 150.0-250.0 DEG C and pressure of 1.0-10.0MPa to generate substituted benzyl cyanide and hydrogen halide, keeping reaction retention time for 10-300s, then cooling for quenching reaction, and post-treating a reaction material to form substituted benzyl cyanide. The method has the advantages of low cost, high production efficiency, continuous production and clean production.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for continuously preparing substituted benzylnitrile compounds using a microchannel reactor. Background technique [0002] Substituted phenylacetonitrile compounds are a very important class of organic intermediates, and their derivatives, substituted phenylacetic acids, are often used in medicine, pesticides and other fields. For example, in the field of medicine, phenylacetic acid and p-methoxyphenylacetic acid are mainly used in the production of penicillin; o-chlorophenylacetic acid is also a raw material for the new anti-inflammatory and analgesic drug diclofenac. In the field of pesticides, 2, 5-dimethylphenylacetonitrile and 2, 4-dichlorophenylacetonitrile are the key intermediates of tetronic acid and other insecticides and acaricides spirotetramat and spirodiclofen, respectively. [0003] There are many methods for preparing substituted phenylacetonit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/14C07C255/33C07C255/35C07C255/37C07C255/42C07C255/36C07C303/22C07C309/59
CPCC07C253/14C07C303/22C07C255/33C07C255/35C07C255/37C07C255/42C07C255/36C07C309/59
Inventor 张辰亮程丽华刘少华董浩浩彭艳丽申银山杨国忠时叶强
Owner HEBEI CHENGXIN
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