Method for continuously synthesizing N,N-diethyl-m-methylbenzamide

A technology of toluamide and toluyl chloride, which is applied in the field of continuous synthesis of N,N-diethyl-m-toluamide, can solve the problem of high requirements for reaction equipment, poor mass and heat transfer effects, and reaction problems. Harsh conditions and other problems, to achieve the effect of shortening the production time of the process, short reaction time, safe and controllable process

Inactive Publication Date: 2018-03-27
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The above method has optimized and improved the synthetic method of N,N-diethyl-m-methylbenzamide from different angles, but there are still some problems to be solved: firstly, the batch process is still mainly used in large-scale production Batch production, low reaction effi

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  • Method for continuously synthesizing N,N-diethyl-m-methylbenzamide
  • Method for continuously synthesizing N,N-diethyl-m-methylbenzamide

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Embodiment 1

[0031] (1) Refer to figure 2 Determine the reactor connection mode, the channel type is (4e+4a) cylindrical straight channel and diamond microchannel structure, the channel volume and flow rate determine the reaction molar ratio, and the heat exchange medium is heat transfer oil.

[0032] 365g (5mol) diethylamine and 1333g aqueous sodium hydroxide solution (15%) are mixed and stirred to form a diethylamine-sodium hydroxide system; m-toluoyl chloride is an acid chloride system, and the two systems are respectively mixed at 30ml / min and The flow velocity of 50ml / min is injected in the reactor by metering pump, and this moment n (m-toluoyl chloride):n (diethylamine)=1:1, adopts figure 2 In a microchannel reactor, the temperature is controlled at 30°C, the residence time is 60s, the reaction liquid is quantitatively collected and separated into a separatory funnel, the organic phase is retained, the aqueous phase is extracted three times with ether, the organic phases are combin...

Embodiment 2

[0034] (1) Refer to figure 2 Determine the reactor connection mode, the channel type is (4e+4b) cylindrical straight channel and heart-shaped microchannel structure, the channel volume and flow rate determine the reaction molar ratio, and the heat exchange medium is heat transfer oil.

[0035] 365g (5mol) diethylamine and 1000g sodium hydroxide aqueous solution (20%) are mixed and stirred to form a diethylamine-sodium hydroxide system; m-toluoyl chloride is an acid chloride system, and the two systems are respectively mixed at 35ml / min and The flow rate of 45ml / min is injected in the reactor by metering pump, and this moment n (m-toluoyl chloride):n (diethylamine)=1:1.2, adopts figure 2 In a microchannel reactor, control the temperature at 35°C and the residence time of 120s. Quantitatively collect the reaction liquid into a separatory funnel for separation, keep the organic phase, extract the water phase with ether three times, combine the organic phases, dry with anhydrous s...

Embodiment 3

[0037] (1) Refer to figure 2 Determine the reactor connection mode, the channel type is (4e+4c) cylindrical straight channel and triangular microchannel structure, the channel volume and flow rate determine the reaction molar ratio, and the heat exchange medium is heat transfer oil.

[0038] 365g (5mol) diethylamine and 800g aqueous sodium hydroxide solution (25%) are mixed and stirred to form a diethylamine-sodium hydroxide system; m-toluoyl chloride is an acid chloride system, and the two systems are respectively mixed at 40ml / min and The flow velocity of 40ml / min is injected in the reactor by metering pump, and this moment n (m-toluoyl chloride):n (diethylamine)=1:2, adopts figure 2 In a microchannel reactor, the temperature is controlled at 40°C, and the residence time is 180s. Quantitatively collect the reaction liquid and transfer it to a separatory funnel for separation. Keep the organic phase, extract the water phase with ether three times, combine the organic phases...

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Abstract

The invention relates to a method for continuously synthesizing N,N-diethyl-m-methylbenzamide, belonging to the technical field of organic synthesis processes. The method is a technology characterizedby taking m-methyl benzoyl chloride and diethylamine as raw materials, taking alkali compounds of metals such as sodium and potassium as acid-binding agents, taking water as a solvent, and preparingthe N,N-diethyl-m-methylbenzamide in a continuous flow microchannel reactor. The method provided by the invention has the advantages of mild conditions, short reaction time, high raw material utilization rate, continuous operation and high production efficiency, can realize effective control in a reaction process, and is safe and stable.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and relates to a method for preparing N,N-diethyl m-toluamide by reacting m-toluyl chloride in a continuous flow microchannel reactor, more specifically, m-toluamide Toluyl chloride and diethylamine are used as substrates, basic compounds of sodium and potassium metals are used as acid-binding agents, and water is used as solvent to react in a continuous flow microchannel reactor to generate N,N-diethyl-m-methyl Benzamide method. Background technique [0002] N,N-diethyl-m-methylbenzamide, referred to as DEET, is one of the amide compounds with a relative molecular weight of 191.27. It is a colorless to light yellow liquid in appearance. Insoluble in water, slightly soluble in petroleum ether, miscible with benzene, ether, ethanol, chloroform, propylene glycol, etc. It is an insect pheromone, which has a repelling effect on mosquitoes and other biting pests. It can be direc...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C233/65B01J19/00
CPCC07C231/02B01J19/002B01J19/0046B01J19/0093B01J2219/00867C07C233/65
Inventor 严生虎程昊张跃刘建武沈介发辜顺林马晓明陈代祥张勇超魏进刘浩沈禹凡
Owner CHANGZHOU UNIV
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