Method for one-step synthesizing N,N-diethyl-m-methyl benzamide in fixed bed

A technology of methyl benzamide and methyl benzoic acid diethylamine salt, which is applied in the field of chemical preparation, can solve the problems of discontinuous synthesis reaction, complex reaction route, and high comprehensive cost, and achieve uniform catalyst distribution and high yield , highly selective effect

Inactive Publication Date: 2009-02-11
JIANGSU PANOXI CHEM
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Problems solved by technology

[0009] The above-mentioned three methods of synthesizing N, N-diethyl-m-methylbenzamide mainly have one or more of the following disadvantages: the synthetic re...

Method used

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  • Method for one-step synthesizing N,N-diethyl-m-methyl benzamide in fixed bed
  • Method for one-step synthesizing N,N-diethyl-m-methyl benzamide in fixed bed
  • Method for one-step synthesizing N,N-diethyl-m-methyl benzamide in fixed bed

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Embodiment Construction

[0029] The present invention is described in detail below in conjunction with specific examples, but the present invention is not limited to these disclosed embodiments, and the present invention will cover the range described in the patent book, and various modifications and equivalent changes of the scope of claims.

[0030] The technical process of embodiment 1-327 is: m-toluic acid and diethylamine are stirred and reacted in a 2000L stainless steel kettle under solvent system to generate m-toluic acid diethylamine salt complex, and then use 2J -x The plunger type metering pump continuously feeds the catalytic fixed bed, dehydrates at constant temperature and pressure to obtain a crude product, distills at atmospheric pressure to recover the solvent, and finally rectifies under reduced pressure to obtain pure N,N-diethyl-m-methylbenzamide Taste.

[0031] Embodiment 1-327 specific process conditions, m-toluic acid: diethylamine: solvent molar ratio, solvent type, catalyst ac...

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Abstract

The invention discloses a one-step synthesis method of N, N-diethyl-3-methyl-benzamide with a fixed bed, which comprises the steps that: 3-methyl benzoic acid and diethylamine are stirred under a solvent system for reaction to generate a complex salt compound of the 3-methyl benzoic acid and diethylamine, and then materials are fed to the catalyzing fixed bed continuously under constant temperature and constant pressure, then dehydrated continuously to obtain a crude product; the solvent is recovered by distillation under ordinary pressure; finally the pure product of the N, N-diethyl-3-methyl-benzamide is obtained after rectification under vacuum. The molar ratio of the 3-methyl benzoic acid to the diethylamine to the solvent is 1.0: (1.0-15.0): (0-25.0), the mass velocity is 0.1 h<-1> to 20.0 h<-1>, the reaction temperature of the fixed bed is 60 DEG C to 550 DEG C and the reaction pressure of the fixed bed is 0.1 MPa to 5.0 MPa. The synthesis technology has the advantages of short technological process, high conversion ratio, good selectivity, high yield rate, small amount of waste gas, waste water and waste residues, reproducible and recyclable catalyst and low cost.

Description

technical field [0001] The invention relates to a method for one-step synthesis of N,N-diethyl-m-toluamide on a fixed bed, belonging to the technical field of chemical preparation. Background technique [0002] Biting pests such as mosquitoes have always brought serious troubles and even disasters to humans. They not only suck human blood, disturb people's peace, but also infect diseases. In order to eliminate the troubles that biting pests bring to humans, people have discovered and synthesized a variety of insect repellents. Among the various insect repellents known at present, N, N-diethyl-m-methylbenzamide is the The one with the broadest spectrum of physiological activity and the most significant comprehensive repellent effect. It not only shows high repellent activity against mosquitoes, but also has repellent effect on other pests, such as cockroaches, fleas, midges, sand fleas, sand mites, etc. . In addition, it is also a safe insect repellent, and it is effective...

Claims

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Application Information

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IPC IPC(8): C07C233/65C07C231/02
CPCY02P20/584
Inventor 朱益民张跃
Owner JIANGSU PANOXI CHEM
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