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Preparation of medicinal D,L-2-hydroxy-4-methylthio calcium butyrate

A technology of calcium methylthiobutyrate and methylthiobutyric acid, which is applied in the field of medicinal D, and achieves the effects of low cost, convenient preparation, and easy control of product quality

Active Publication Date: 2009-01-21
NANJING LIFENERGY R & D +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the distillation step in this invention must be equipped with a high-vacuum glass thin-film evaporator, and the pressure required to reach below 20Pa can ensure that the HMBA obtained by distillation does not contain or contain very low concentrations of dimers and oligomers. Such a high vacuum requirement, At present, it is only possible to achieve this kind of experimental scale equipment.

Method used

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  • Preparation of medicinal D,L-2-hydroxy-4-methylthio calcium butyrate
  • Preparation of medicinal D,L-2-hydroxy-4-methylthio calcium butyrate

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Embodiment 1: D, the preparation of L-2-hydroxyl-4-methylthiobutyric acid methyl ester

[0024] Add 60g of Alimet to a 500mL three-neck round bottom flask with mechanical stirring TM (NOVUS company), start stirring, add 120mL ethyl acetate, stir for about 5 minutes, add 120mL water; continue stirring for about 5 minutes, transfer the liquid in the flask to a separatory funnel, take the upper layer of ethyl acetate and evaporate it under reduced pressure to recover acetic acid ethyl ester to obtain 48.9 g of a dark brown concentrated solution.

[0025] In another 500mL three-neck round bottom flask with magnetic stirring and reflux condenser, add 45.1g of the above concentrated solution and 121.4mL of methanol, start stirring, add 15g of sulfuric acid (concentration: 98%), heat to reflux, and the reaction ends after 4h; Cool, evaporate under reduced pressure to recover methanol, add 90mL ethyl acetate to the concentrated solution to dilute, wash the diluted solution wit...

Embodiment 2

[0026] Embodiment 2: D, the preparation of L-2-hydroxyl-4-methylthiobutyric acid methyl ester

[0027] Add 60g of Alimet to a 500mL three-neck round bottom flask with mechanical stirring TM (NOVUS company), start stirring, add 120mL ethyl acetate, stir for about 5 minutes, add 120mL water; continue stirring for about 5 minutes, transfer the liquid in the flask to a separatory funnel, take the upper layer of ethyl acetate and evaporate it under reduced pressure to recover acetic acid ethyl ester to obtain 47.6 g of a dark brown concentrated solution.

[0028] In another 500mL three-necked round bottom flask with magnetic stirring and reflux condenser, add 45.1g of the above concentrated solution and 242.7mL of methanol, start stirring, add 12g of sulfuric acid (concentration: 98%), heat to reflux, and the reaction ends after 4h; Cool, evaporate under reduced pressure to recover methanol, add 90mL ethyl acetate to the concentrated solution to dilute, wash the diluted solution w...

Embodiment 3

[0029]Embodiment 3: D, the preparation of L-2-hydroxyl-4-methylthiobutyric acid methyl ester

[0030] Add 60g of Alimet to a 500mL three-neck round bottom flask with mechanical stirring TM (NOVUS company), start stirring, add 120mL ethyl acetate, stir for about 5 minutes, add 120mL water; continue stirring for about 5 minutes, transfer the liquid in the flask to a separatory funnel, take the upper layer of ethyl acetate and evaporate it under reduced pressure to recover acetic acid ethyl ester to obtain 48.3 g of a dark brown concentrated solution.

[0031] In another 500mL three-necked round bottom flask with magnetic stirring and reflux condenser, add 45.1g of the above concentrate and 364mL of methanol, start stirring, add 9g of sulfuric acid (concentration is 98%), heat to reflux, and the reaction ends after 5h; cooling , methanol was recovered by evaporation under reduced pressure, the concentrated solution was diluted with 90mL ethyl acetate, and the diluted solution wa...

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Abstract

The invention discloses a method for preparing a D, L-2-hydroxyl-4-methylthio butanoic calcium salt for medicinal purpose. The method comprises following steps of: a. using a D,L-2-hydroxyl-4-methylthio butanoic acid and an alcohol with a general formula of ROH as the raw materials to carry out esterification to obtain a D, L-2-hydroxyl-4-methylthio butyrate, and; b. hydrolyzing the D, L-2-hydroxyl-4-methylthio butyrate in step a and calcium oxide in a solvent to produce the D, L-2-hydroxyl-4-methylthio butanoic calcium salt. The method provided by the invention for the production of the D, L-2-hydroxyl-4-methylthio butanoic calcium salt has the advantages of short course, readily available the raw materials, low cost, easy control over the quality of the product, and more importantly, the method can prepare high-purity D, L-2-hydroxyl-4-methylthio butanoic calcium salt for medicinal purpose, thereby satisfying the requirements of State Food and Drug Administration Bureau and Good Manufacturing Practice (GMP) for drug production, and facilitating the preparation of pharmaceutical preparations.

Description

technical field [0001] The present invention relates to a preparation method of pharmaceutical D, L-2-hydroxy-4-methylthiobutyrate calcium (HMBC), in particular, the present invention relates to a two-stage process, which comprises esterification of D, L- 2-Hydroxy-4-methylthiobutyric acid, and then the esterification product is hydrolyzed into a salt. Background technique [0002] D, Calcium L-2-hydroxy-4-methylthiobutyrate is the calcium salt of the racemic hydroxy analog of the basic amino acid methionine, which is an important additive not only in poultry feeding, but also in many other feeding fields additive. In addition, studies have demonstrated that calcium D,L-2-hydroxy-4-methylthiobutyrate has medicinal uses as an alternative or supplement to dialysis therapy in the treatment of renal failure. [0003] Calcium D, L-2-hydroxy-4-methylthiobutyrate currently in commercial use (the main product Elemis Calcium, MHA ), the technically unique synthetic route is to st...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/20
Inventor 陈爱军杨洁熊守军李德富黄安民
Owner NANJING LIFENERGY R & D
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