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Micro-reaction continuous flow synthesis method of levocarnitine

A technology of micro-reaction and micro-channel reactor, applied in the direction of organic chemical method, cyanide reaction preparation, chemical instrument and method, etc., can solve the problems of many side reactions, low yield, long reaction time, etc., and achieve simple operation, Increased product yield and low cost

Active Publication Date: 2020-08-28
FUDAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is that in the existing levocarnitine preparation process, the traditional batch-type trimethylamine quaternization reaction time is long, the side reactions are many and the yield is low, and a micro-reaction continuous flow Synthetic method, the reaction time of this method is greatly shortened, the product yield is significantly improved, the operation is simple and convenient, and it is easy to industrialized production

Method used

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  • Micro-reaction continuous flow synthesis method of levocarnitine
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  • Micro-reaction continuous flow synthesis method of levocarnitine

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Embodiment 1

[0043] The microchannel reactor adopts a 316L stainless steel microtubular reactor with an outer diameter of 1.6 mm, an inner diameter of 1.0 mm, and a total volume of 7.85 ml. For the reaction process, see figure 1 .

[0044]Firstly prepare an aqueous sodium hydroxide solution with a concentration of 4.77% by mass and an aqueous solution of hydrochloric acid with a concentration of 10% by mass, then pass trimethylamine gas into the aqueous solution of sodium hydroxide to prepare a solution with a concentration of 12% by mass. Trimethylamine aqueous solution. The trimethylamine aqueous solution and the substrate (R)-(+)-4-chloro-3-hydroxybutyrate ethyl ester are simultaneously pumped into the micro-mixer (3), and the volume flows of the two materials are adjusted respectively so that the substrate and the trimethylamine The mol ratio is 0.25, and two strands of materials are mixed in the micro-mixer (3), then enter the micro-channel reactor (4), the temperature in the micro-...

Embodiment 2

[0046] The microchannel reactor adopts a polytetrafluoroethylene (PTFE) microtubular reactor with an outer diameter of 1.6 mm, an inner diameter of 0.9 mm, and a total volume of 9.54 ml. For the reaction process, see figure 1 .

[0047] First prepare the aqueous sodium hydroxide solution with a mass percentage concentration of 6.34% and the hydrochloric acid aqueous solution with a mass percentage concentration of 8%, then pass trimethylamine gas into the above-mentioned aqueous sodium hydroxide solution to prepare a 15% aqueous solution of Trimethylamine aqueous solution. The trimethylamine aqueous solution and the substrate (R)-(+)-4-chloro-3-hydroxybutyrate ethyl ester are simultaneously pumped into the micro-mixer (3), and the volume flows of the two materials are adjusted respectively so that the substrate and the trimethylamine The mol ratio is 0.3, and the two stocks of materials are mixed in the micro-mixer (3), then enter the micro-channel reactor (4), the temperatu...

Embodiment 3

[0049] The microchannel reactor adopts a 304 stainless steel microtubular reactor with an outer diameter of 3.2 mm, an inner diameter of 2.2 mm, and a total volume of 38 ml. For the reaction process, see figure 1 .

[0050] First prepare the aqueous sodium hydroxide solution with a mass percentage concentration of 3.6% and the hydrochloric acid aqueous solution with a mass percentage concentration of 7%, then pass trimethylamine gas into the above-mentioned aqueous sodium hydroxide solution, and prepare a 8% hydrochloric acid solution with a mass percentage concentration of Trimethylamine aqueous solution. The trimethylamine aqueous solution and the substrate (R)-(+)-4-chloro-3-hydroxybutyrate ethyl ester are simultaneously pumped into the mixer (3), and the volume flows of the two stocks of materials are adjusted respectively so that the substrate and the trimethylamine The molar ratio is 0.32. The two materials are mixed in the micro-mixer (3), and then enter the micro-ch...

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Abstract

The invention provides a micro-reaction continuous flow synthesis method of levocarnitine. An existing preparation method has the defects of complicated operation, long reaction time, low yield and the like. According to the method, (R)-4-halogenated-3-hydroxybutyrate and trimethylamine are continuously subjected to quaternization and hydrolysis reaction in a micro-channel reactor in the presenceof an alkali to prepare the levocarnitine. The reaction time of the method is only several minutes, the yield is high, the technological process is easy and convenient to operate, and industrial production is easy.

Description

technical field [0001] The present invention relates to the synthesis of levocarnitine (I), in particular to a micro-reaction continuous flow synthesis method of levocarnitine. [0002] Background technique [0003] L-Carnitine (I), also known as L-carnitine, vitamin B T , is a key transmitter in the process of fat metabolism, and its main function is to promote the oxidative decomposition of fatty acids into the mitochondria to provide energy for cells. It is widely used, and can be used for carnitine deficiency, treatment of various ischemic heart diseases, liver diseases, kidney diseases and muscle movement disorders, etc., and can also be used as food additives and feed additives. WO 2007 / 139238, US 4895979, EP 0339764, and JP 1989211551 all describe the quaternization of (R)-4-halo-3-hydroxybutyrate and 27-30% trimethylamine aqueous solution in the aqueous phase, and then The method for preparing (I) by hydrochloric acid hydrolysis. Although the reaction time of t...

Claims

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Application Information

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IPC IPC(8): C07C229/22C07C227/08B01J19/00
CPCC07C227/08B01J19/0093C07B2200/07B01J2219/00961B01J2219/00963B01J2219/00984C07C229/22B01J2219/00795B01J2219/0086B01J2219/00869B01J2219/00889C07C227/04
Inventor 陈芬儿刘敏杰程荡姜梅芬王泽旭黄则度王佳琦
Owner FUDAN UNIV
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