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Method for preparing N,N-dipropyl m-methylbenzamide

A technology of toluamide and m-toluyl chloride, which is applied in the field of organic compound preparation, can solve the problems of unfavorable economic benefits, difficulty in reducing costs, and low production efficiency, so as to reduce production costs, realize simple implementation, and facilitate operation Effect

Inactive Publication Date: 2018-03-20
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The usual production method of N,N-dipropyl-m-methylbenzamide is direct amidation reaction, absorbing organic amine as acid, and the color of the product obtained is darker, which is difficult to sell as a product, and must be further refined, that is, reduced Pressure refining treatment steps, the problems of this type of preparation method: 1, because need to use expensive high-vacuum pump to realize in the vacuum refining treatment step, therefore, this method exists the problem of many production equipments, high cost, thus it is difficult to reduce cost
2. Since the vacuum refining treatment step is an indispensable and time-consuming production step in the production of N,N-dipropyl-m-methylbenzamide, the method has the problems of long production time and low production efficiency , is not conducive to the improvement of the economic efficiency of enterprises

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] This preparation N, the method for N-dipropyl m-toluamide comprises the following steps:

[0024] ⑴ amidation reaction steps

[0025] Add 128 kg of dipropylamine, 40 kg of water, and 125 kg of benzene into a 500-liter reactor with a cooling device, electric stirring, and a thermometer. Under stirring, add 100 kg of m-toluyl chloride and compound acid absorption at the same time. Refined preparation (sodium carbonate, potassium carbonate) 45 kilograms, keep room temperature reaction, material is added, stir reaction until no bubble escapes, and reaction is completed.

[0026] ⑵Washing steps

[0027] Add 40 kg of water to the oil-layer mixture obtained after the amidation reaction, stir evenly, leave to separate layers, and remove the water layer therein.

[0028] (3) Distillation and desolventization step

[0029] The remaining liquid obtained by distilling and desolventizing benzene from the mixed solution washed with water is the finished product of N,N-dipropyl m-t...

Embodiment 2

[0031] This N, the preparation method of N-dipropyl m-toluamide comprises the following steps:

[0032] (1) Put 50 kg of propylenediamine, 65 kg of water, and 250 kg of benzene into a 500-liter reaction kettle with a cooling device, electric stirring, and a thermometer. Under stirring, add 160 kg of m-toluyl chloride and acid Absorb 46 kilograms of refined preparations (sodium carbonate, potassium carbonate), keep room temperature for reaction, add materials, stir and react for 1.5 hours, and the reaction is completed.

[0033] ⑵Washing steps

[0034] Add 40 kg of water to the oil-layer mixture obtained after the amidation reaction, stir evenly, leave to separate layers, and remove the water layer therein.

[0035] (3) Distillation and desolventization step

[0036] The remaining liquid obtained by distilling and desolventizing benzene from the mixed solution washed with water is the finished product of N,N-dipropyl m-toluamide. The content of N,N-dipropyl m-toluamide is 98....

Embodiment 3

[0038] This N, the preparation method of N-dipropyl m-toluamide comprises the following steps:

[0039] ⑴ amidation reaction steps

[0040] Add 128 kg of dipropylamine, 40 kg of water, and 125 kg of benzene into a 500-liter reactor with a cooling device, electric stirring, and a thermometer. Under stirring, add 100 kg of m-toluyl chloride and compound acid absorption at the same time. Refining agent (sodium carbonate, potassium carbonate) 35 kilograms, keep room temperature reaction, material is added, stir reaction until no bubble escapes, and reaction is finished.

[0041] ⑵Washing steps

[0042] Add 40 kg of water to the oil-layer mixture obtained after the amidation reaction, stir evenly, leave to separate layers, and remove the water layer therein.

[0043] (3) Distillation and desolventization step

[0044] The remaining liquid obtained by distilling and desolventizing benzene from the mixed solution washed with water is the finished product of N,N-dipropyl m-toluamid...

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PUM

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Abstract

The invention relates to a method for preparing N,N-dipropyl-m-toluamide. The method comprises the following steps: (1) amidation reaction step, dipropylamine, benzene and water are put into a reaction kettle, stirred, and simultaneously separated into Add m-toluoyl chloride and compound acid in batches to absorb the refined preparations sodium carbonate and potassium carbonate, keep the reaction at room temperature, and complete the addition of materials, stir the reaction until no bubbles escape, and the reaction is completed; (2) washing step, the mixture after amidation reaction Add water to the medium, stir evenly, stand for stratification, and remove the water layer therein; (3) distillation and desolvation step. The compound acid absorption refined preparation used in the preparation method of this N,N-dipropyl-m-toluamide is sodium carbonate and potassium carbonate, which have the characteristics of low price and easy procurement.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a simple and effective preparation method of N,N-dipropyl m-toluamide. Background technique [0002] In industrial production and cosmetics industrial production, N,N-dipropyl m-toluamide is used more and more widely as an important organic compound and additive. The usual production method of N,N-dipropyl-m-methylbenzamide is direct amidation reaction, absorbing organic amine as acid, and the color of the product obtained is darker, which is difficult to sell as a product, and must be further refined, that is, reduced Pressure refining treatment steps, the problems of this type of preparation method: 1, because need to use expensive high-vacuum pump to realize in the vacuum refining treatment step, therefore, this method exists the problem of many production equipments, high cost, thus it is difficult to reduce cost . 2. Since the vacuum refining treatment step is a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C231/24C07C233/65
CPCC07C231/02C07C231/24C07C233/65
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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