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Method for continuously preparing (R)-4-halo-3-hydroxy-butyrate by using micro-reaction system

A micro-reaction, butyrate technology, applied in biochemical equipment and methods, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of slowing down the reaction rate, affecting the selectivity of the reaction, and low yield, etc. Achieve the effect of high degree of automation, improved product yield and shortened reaction time

Active Publication Date: 2021-02-02
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Poor multiphase mass transfer and mixing performance and wide droplet size distribution in the batch reactor not only affect the progress of the reaction process and the selectivity of the reaction, but also slow down the reaction rate, which leads to long reaction time, low efficiency and low efficiency of the enzyme-catalyzed method. One of the important reasons for the low yield

Method used

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  • Method for continuously preparing (R)-4-halo-3-hydroxy-butyrate by using micro-reaction system
  • Method for continuously preparing (R)-4-halo-3-hydroxy-butyrate by using micro-reaction system
  • Method for continuously preparing (R)-4-halo-3-hydroxy-butyrate by using micro-reaction system

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Experimental program
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Effect test

Embodiment 1

[0070] This embodiment provides a method for continuously preparing (R)-4-chloro-3-hydroxy-butyric acid ethyl ester using a micro-reaction system, such as figure 2 Shown, comprise the micromixer 10 that communicates successively, microchannel reactor 11, pH regulator 14, microchannel reactor 17, pH regulator 19, microchannel reactor 22, pH regulator 24, back pressure valve 26, The product liquid collection storage tank 27 also includes a computer 16, a pH meter body 21, a pH measuring probe 15, a pH measuring probe 20, a pH measuring probe 25, a pH regulator delivery pump 13, a pH regulator delivery pump 18, a pH regulator Delivery pump 23 and pH regulator storage tank 12.

[0071] The pH measuring meter body 21 , the pH measuring probe 15 , the pH measuring probe 20 and the pH measuring probe 25 form a pH measuring meter.

[0072] The computer 16, the pH meter body 21, the pH measuring probe 15, the pH measuring probe 20, the pH measuring probe 25, the pH regulator delivery...

Embodiment 2

[0085] The micro-reaction system used in this embodiment, the experimental operation steps, methods and conditions are all the same as in Example 1, the only difference is that the pH value of the reaction mixture in the pH regulator 14, the pH regulator 19 and the pH regulator 24 is determined by The pH automatic adjustment system is stably controlled at 7.0.

[0086] Sampling and analysis were performed by Agilent liquid chromatography for quantitative detection, and the concentration of reaction substrate and product was quantified by peak area. After analysis, the reaction substrate ethyl chloroacetoacetate was completely converted, and the yield of the product (R)-4-chloro-3-hydroxybutyric acid ethyl ester was 98.7%.

Embodiment 3

[0088] The micro-reaction system used in this embodiment, the experimental operation steps, methods and conditions are all the same as in Example 1, the only difference is that the pH value of the reaction mixture in the pH regulator 14, the pH regulator 19 and the pH regulator 24 is determined by The pH automatic adjustment system is stably controlled at 6.2.

[0089] Sampling and analysis were performed by Agilent liquid chromatography for quantitative detection, and the concentration of reaction substrate and product was quantified by peak area. After analysis, the reaction substrate ethyl chloroacetoacetate was completely converted, and the yield of the product (R)-4-chloro-3-hydroxybutyric acid ethyl ester was 95.4%.

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Abstract

The invention belongs to the technical field of chemical engineering, and particularly relates to a method for continuously preparing (R)-4-halo-3-hydroxy-butyrate by using a micro-reaction system. Asubstrate solution containing halogenated acetoacetate and a biological catalytic solution are continuously subjected to an enzyme-catalyzed asymmetric reduction reaction in the micro-reaction systemcomposed of a micro-mixer, a micro-channel reactor and a pH regulator so as to obtain the (R)-4-halo-3-hydroxy-butyrate. Compared with the prior art, the method has the advantages that: the reaction time is only a few minutes, the yield of the product (R)-4-halo-3-hydroxy-butyrate is more than 95 percent, the process is continuous, the automation degree is high, the efficiency is high, the technological process is simple and convenient to operate, and the industrial production is easy.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for continuously preparing (R)-4-halo-3-hydroxy-butyrate using a micro-reaction system. Background technique [0002] (R)-4-halo-3-hydroxy-butyrate is a key intermediate in the synthesis of L-carnitine. The preparation of (R)-4-halo-3-hydroxy-butyrate by asymmetric catalytic reduction from haloacetoacetate is the most efficient way of atom economy. Kitamura et al. ( Tetrahedron Letters , 1988, 29, 1555-1556) reported the preparation of (R)-4-halogenated -3-hydroxy-butyrate method, although this method can reach 97% ee value (i.e. enantiomeric excess enantiomeric excess percentage), but the catalyst and ligand preparation process is complicated, S / C value (i.e. substrate / catalyst The ratio of substrate to catalyst) is low, the cost is high, and high temperature and high pressure reaction conditions are required, the operation is complicated, and t...

Claims

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Application Information

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IPC IPC(8): C07C67/31C07C69/675B01J19/00
CPCC07C67/31B01J19/0093C07C69/675C12Y101/01184C12P7/62C12M21/18C12M23/16C12M23/06C12M27/00B01J2219/00889B01J2219/00783B01J2219/00792B01F33/30B01F25/31422C12M23/58C12M29/00C12M41/12C12M41/26C12M41/48C12P7/625
Inventor 陈芬儿程荡黄则度刘敏杰黄华山姜梅芬王路路
Owner FUDAN UNIV
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