Method for preparing ethyl lipoate by virtue of tubular reactor

A technology of tubular reactor and ethyl lipoic acid, which is applied in chemical instruments and methods, chemical/physical/physical chemical fixed reactors, chemical/physical/physical chemical processes, etc., can solve the problem of shortening reaction time and heat preservation reaction Long time, uncontrollable temperature and other problems, to achieve the effect of shortening the reaction time, improving the yield and quality, and controlling the temperature

Inactive Publication Date: 2018-11-09
SUZHOU FUSHILAI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a method for preparing ethyl lipoic acid using a tubular reactor, which overcomes the uncontrollable temperature in the prior art, adding hydrosulfite for 1.5 hours of heat preservation, long heat preservation reaction time, and low yield. , the reaction method has good heat exchange effect, reduces ester group hydrolysis, reduces reaction steps, shortens reaction time, improves product quality, and increases reaction yield

Method used

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  • Method for preparing ethyl lipoate by virtue of tubular reactor
  • Method for preparing ethyl lipoate by virtue of tubular reactor
  • Method for preparing ethyl lipoate by virtue of tubular reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Preparation of raw material 1 (sodium disulfide): In a 500ml three-necked reaction flask, put sulfur: 30 grams, 400 grams of water, and sodium sulfide pentahydrate: 150 grams, control the internal temperature at 40-50 degrees, and stir to obtain a clear liquid. It weighs 580 grams and is ready to use. (The pump used is metering pump 1)

[0038] Preparation of raw material 2 (ethyl 6,8-dichlorooctanoate): 97.5% of ethyl 6,8-dichlorooctanoate: 200 grams. stand-by. (The pump used is metering pump 2)

[0039] Using liquid-liquid two-phase reaction:

[0040] Set the flow rate of metering pumps 3 and 4 and pump them into the tubular reactor to complete the reaction of raw material 1 and raw material 2 at the same time. That is, the flow rate of raw material 1 is 5.80 g / sec, that is, the flow rate of raw material 2 is 2.0 g / sec. The reaction temperature is controlled to 40°C, the reaction residence time is 30 seconds, and the reaction product is collected. After all the product...

Embodiment 2

[0044] The raw material 1 and raw material 2 in Example 1 were used.

[0045] Set the flow rate of metering pumps 3 and 4 and pump them into the tubular reactor to complete the reaction of raw material 1 and raw material 2 at the same time. That is, the flow rate of raw material 1 is 5.80 g / sec, that is, the flow rate of raw material 2 is 2.0 g / sec. The reaction temperature is controlled at 60°C, the reaction residence time is 36 seconds, and the reaction product is collected. After all the products are collected, they are extracted with toluene. After the toluene is evaporated on a rotary evaporator, 197.80 grams are weighed. The content of ethyl lipoic acid in the product was 95.65%, and the yield was 96.41%.

Embodiment 3

[0047] Raw material 1: Preparation of (sodium sulfide): 300 grams of water and 150 grams of sodium sulfide pentahydrate in a 500m beaker, the internal temperature is controlled at 50 degrees, and the mixture is stirred to obtain a clear liquid, with a total weight of 450 grams, ready for use. (The pump used is metering pump 1)

[0048] Preparation of raw material 2 (sulfur powder and solid suspension of ethyl 6,8-dichlorooctanoate): 30 grams of sulfur powder and 97.5% of ethyl 6,8-dichlorooctanoate: 200 grams, total weight 230 grams. In the stirring beaker, keep stirring to evenly distribute the sulfur in the liquid, and set aside. (The pump used is metering pump 2)

[0049] Solid-liquid two-phase reaction:

[0050] Set the flow rate of metering pumps 3 and 4 and pump them into the tubular reactor to complete the reaction of raw material 1 and raw material 2 at the same time. That is, the flow rate of raw material 1 is 4.50 g / sec, that is, the flow rate of raw material 2 is 2.30 g...

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PUM

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Abstract

The invention relates to a method for preparing ethyl lipoate by virtue of a tubular reactor. The method comprises the steps of respectively injecting the raw materials into the tubular reactor for reaction, controlling the reaction temperature to be 40-60 DEG C and the reaction standing time to be 8-36 seconds, and after the reaction is finished, carrying out collection and purification, so as toobtain ethyl lipoate. According to the method, the preparation defects in the prior art are overcome, the heat exchange effect of the reaction is good, the hydrolysis of ester groups is reduced, thereaction time is shortened, the product quality is improved, and the reaction yield is increased.

Description

Technical field [0001] The invention belongs to the field of preparation of ethyl lipoic acid, and particularly relates to a method for preparing ethyl lipoic acid by adopting a tubular reactor. Background technique [0002] The existing preparation process of ethyl lipoic acid is that the main raw material, ethyl 6,8-dichlorooctanoate is put into the reaction kettle, and sodium disulfide is added dropwise; or ethyl 6,8-dichlorooctanoate and sulfur are put into the reaction kettle, Sodium sulfide was added dropwise for about 5 hours or more. After the dropwise addition, sodium sulfide was added and kept for 1.5 hours to obtain ethyl lipoic acid, which was put into the next reaction. [0003] The defects of the existing preparation process are as follows: (1) In the kettle reaction, when sodium sulfide or sodium disulfide is added dropwise, there is a violent exothermic phenomenon, and the temperature is uncontrollable; (2) while the dropwise addition generates heat, it will Impuri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D339/04B01J19/24
CPCB01J19/0013B01J19/2415C07D339/04B01J2219/00074
Inventor 谭雪良丁建飞唐欢
Owner SUZHOU FUSHILAI PHARMA CO LTD
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