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Method for preparing N,N-diethyl M-Methyl Benzoyl amide

A technology of methyl benzamide and methyl benzoyl chloride, applied in the N field, can solve the problems of many impurities, long production time, and many production equipment, and achieve the effects of wide source of raw materials, improved production efficiency and low price

Inactive Publication Date: 2010-12-15
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

N, the usual production method of N-diethyl m-toluamide is direct amidation reaction, with organic amine as acid absorbent, the problems that this kind of preparation method exists: 1, the product color that makes is darker, impurity More, it is difficult to sell as a product, and it must be further refined before it can be used as a raw material, such as vacuum refining treatment, etc. Expense is high, it is difficult to reduce cost; 3, because decompression refining treatment step is to produce N in the process of N, N-diethyl-m-methylbenzamide indispensable and very time-consuming production step, this method also has long production time , the problem of low production efficiency
[0004] After comparison, the above-mentioned patent and the present application all have increased differences in both the reaction temperature and the reaction steps.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A kind of N, the preparation method of N-diethyl m-toluamide, the steps are as follows:

[0021] (1) amidation reaction step

[0022] Put 80 kg of ethylenediamine, 104 kg of water, and 200 kg of benzene into a 500-liter reactor equipped with a cooling device, electric stirring, and a thermometer. While stirring, add 160 kg of m-toluyl chloride and acid absorption Refining preparation sodium hydroxide 46 kilograms, keep room temperature reaction, material is added, and stirring reaction 1.5 hours, reaction completes;

[0023] Mid-term: the weight ratio of acid absorption refined preparation: m-toluoyl chloride is 0.28-0.35:1;

[0024] The weight ratio of m-toluoyl chloride: diethylamine: water: benzene is 1:0.5:0.65:1.25.

[0025] (2) Washing step

[0026] Add 40 kilograms of washing water to the oil layer mixed solution obtained after the amidation reaction, stir evenly, leave to stand for layering, and remove the water layer therein;

[0027] The weight ratio of wa...

Embodiment 2

[0031] A kind of N, the preparation method of N-diethyl m-toluamide, the steps are as follows:

[0032] (1) amidation reaction step

[0033] Put 80 kg of ethylenediamine, 104 kg of water, and 200 kg of benzene into a 500-liter reactor equipped with a cooling device, electric stirring, and a thermometer. While stirring, add 160 kg of m-toluyl chloride and acid absorption Refining agent sodium hydroxide 48 kilograms, keep room temperature reaction, material is added, and stirring reaction 1.5 hours, reaction is finished;

[0034] (2) Washing step

[0035] Add 40 kilograms of washing water to the oil layer mixed solution obtained after the amidation reaction, stir evenly, leave to stand for layering, and remove the water layer therein;

[0036] (3) distillation desolventization step

[0037] Distill the washed mixed liquid to remove the solvent benzene, the distillation temperature is below 85°C and the vacuum degree is 10-15mmHg, and the remaining liquid is N, N-diethyl-m-met...

Embodiment 3

[0039] A kind of N, the preparation method of N-diethyl m-toluamide, the steps are as follows:

[0040] (1) amidation reaction step

[0041] Put 80 kg of ethylenediamine, 104 kg of water, and 200 kg of benzene into a 500-liter reactor equipped with a cooling device, electric stirring, and a thermometer. While stirring, add 160 kg of m-toluyl chloride and acid absorption 50 kilograms of refined preparation sodium hydroxide, keep room temperature reaction, material is added, and stirring reaction 1.5 hours, reaction completes;

[0042] (2) Washing step

[0043] Add 40 kilograms of washing water to the oil layer mixed solution obtained after the amidation reaction, stir evenly, leave to stand for layering, and remove the water layer therein;

[0044] (3) distillation desolventization step

[0045] Distill the washed mixed liquid to remove the solvent benzene, the distillation temperature is below 85°C and the vacuum degree is 10-15mmHg, and the remaining liquid is N, N-diethyl...

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PUM

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Abstract

The invention relates to a method for preparing N,N-diethyl M-Methyl Benzoyl amide. The method comprises the steps of: orderly adding ethidene diamine, water and benzol in a reactor, stirring and adding M-Methyl Benzoyl formyl chloride and acid absorbing fine preparation, maintaining reaction under a room temperature, stirring and reacting for 1 to 5 hours after completely adding materials, adding water to wash after finishing reaction, stirring, layering, removing water layer, distilling, removing solvent benzol so as to obtain the products of N,N-diethyl M-Methyl Benzoyl amide. In the amidation step of the method, sodium hydroxide is used as acid absorbing fine preparation so as to obtain the produces with high purity and shallow color. The product can be sold without high vacuum refining. The quality of the product totally meets the demand of technical index.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a preparation method of N,N-diethyl-m-toluamide. Background technique [0002] In industrial production and cosmetics industrial production, N, N-diethyl-m-toluamide is used more and more widely as an important organic compound and additive. N, the usual production method of N-diethyl m-toluamide is direct amidation reaction, with organic amine as acid absorbent, the problems that this kind of preparation method exists: 1, the product color that makes is darker, impurity More, it is difficult to sell as a product, and it must be further refined before it can be used as a raw material, such as vacuum refining treatment, etc. Expense is high, it is difficult to reduce cost; 3, because decompression refining treatment step is to produce N in the process of N, N-diethyl-m-methylbenzamide indispensable and very time-consuming production step, this method also has long prod...

Claims

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Application Information

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IPC IPC(8): C07C233/65C07C231/02
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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