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Method for preparing and purifying calcium beta-hydroxy-beta-methylbutyrate

A technology of calcium methylbutyrate and a purification method, which is applied in the field of organic compound preparation, can solve the problems of side reactions, low yield, low purity of β-hydroxy-β-methylbutyrate calcium, etc., and achieves the improvement of product content, Improve efficacy, crystal purity and high yield

Inactive Publication Date: 2018-09-21
JIANGSU XIXIN VITAMIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent application number is 02151042.3, which is mainly prepared by haloform reaction, but diacetone alcohol is mainly used as the reaction raw material in this preparation method, which is easy to cause various side reactions in the reaction, and the prepared β-hydroxy-β-methylbutyrate calcium Low purity, low yield, needs to be improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In the present embodiment, a method for preparing and purifying calcium β-hydroxy-β-methylbutyrate comprises the following steps:

[0023] Step 1) Haloform reaction: Add 100 parts by weight of sodium hypochlorite to the three-necked flask, then cool it to 0°C with ice-salt water, stir and add 20 parts by weight of diacetone alcohol and slowly drop it into the three-necked flask, and keep it warm for 9 hours after the dropwise addition The reaction is complete;

[0024] Step 2) Acidification: Pour the reacted material into the separatory funnel and let it stand for 30 minutes, release chloroform from the bottom valve of the separatory funnel, open the hydrochloric acid drip valve and slowly add hydrochloric acid, and continuously check the pH value until the pH is 2 ;

[0025] Step 3) Extraction: Add ethyl acetate to the acidified solution in batches, add 100 parts by weight of ethyl acetate each time for extraction 5 times, and vacuum concentrate the ethyl acetate laye...

Embodiment 2

[0030] A preparation and purification method of β-hydroxy-β-methylbutyrate calcium, comprising the following steps:

[0031] Step 1) Haloform reaction: Add 100 parts by weight of sodium hypochlorite to the three-necked flask, then cool it to 0°C with ice-salt water, stir and add 20 parts by weight of diacetone alcohol and slowly drop it into the three-necked flask, and keep warm for 10 hours after the dropwise addition The reaction is complete;

[0032] Step 2) Acidification: Pour the reacted material into the separatory funnel and let it stand for 30 minutes, release chloroform from the bottom valve of the separatory funnel, open the hydrochloric acid drip valve and slowly add hydrochloric acid, and continuously check the pH value until the pH is 2.5 ;

[0033] Step 3) Extraction: Add ethyl acetate to the acidified solution in batches, add 100 parts by weight of ethyl acetate each time for extraction 6 times, and vacuum concentrate the ethyl acetate layer extracted each time...

Embodiment 3

[0038] A preparation and purification method of β-hydroxy-β-methylbutyrate calcium, comprising the following steps:

[0039] Step 1) Haloform reaction: Add 100 parts by weight of sodium hypochlorite to the three-necked flask, then cool it to 0°C with ice-salt water, stir and add 20 parts by weight of diacetone alcohol and slowly drop it into the three-necked flask, and keep warm for 12 hours after the dropwise addition The reaction is complete;

[0040] Step 2) Acidification; Pour the reacted material into the separatory funnel and let it stand for 30 minutes, release chloroform from the bottom valve of the separatory funnel, open the hydrochloric acid drip valve and slowly add hydrochloric acid, and continuously check the pH value until the pH is 3 ;

[0041] Step 3) Extraction: Add ethyl acetate to the acidified solution in batches, add 100 parts by weight of ethyl acetate each time for extraction 6 times, and vacuum concentrate the ethyl acetate layer extracted each time u...

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Abstract

The invention discloses a method for preparing and purifying calcium beta-hydroxy-beta-methylbutyrate. The method comprises the following steps: performing haloform reaction by taking sodium hypochlorite as a reaction raw material and diacetone alcohol as a solvent, then performing acidification and ethyl acetate extraction, salifying beta-hydroxy-beta-methyl butyric acid in an ethyl acetate extract and calcium hydroxide and purifying through a cryogenic kettle and a plate and frame filter press to prepare the calcium beta-hydroxy-beta-methylbutyrate. The method disclosed by the invention hasthe advantages of being simple in production process, safe, non-toxic, cheap, convenient to recover and high in crystal purity and yield; meanwhile, a large number of impurities are removed through plate and frame separation, so that the product content is improved, the efficacy is improved, and the labor cost is reduced.

Description

technical field [0001] The invention relates to the technical field of organic compound preparation, in particular to a preparation and purification method of β-hydroxy-β-methylbutyrate calcium (HMB-Ca). Background technique [0002] The compound β-hydroxy-β-methylbutyrate calcium, referred to as HMB-Ca, CAS: 135236-72-5, β-hydroxy-β-methylbutyric acid (HMB) is widely found in citrus fruits, some vegetables such as Cauliflower, legumes such as alfalfa, and certain fish and seafood. [0003] HMB-Ca can be used to promote muscle growth, enhance immunity, reduce the level of cholesterol and low-density lipoprotein (LDL) in the body to reduce the occurrence of coronary heart disease and cardiovascular disease, and can also enhance the body's ability to fix nitrogen and maintain protein levels in the body. It is widely used . [0004] In the prior art, free radical reaction and haloform reaction are mainly used to complete calcium β-hydroxy-β-methylbutyrate. The patent applica...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C51/093C07C51/02C07C51/43C07C51/487C07C51/48C07C59/01
CPCC07C51/02C07C51/093C07C51/412C07C51/43C07C51/48C07C51/487C07C59/01
Inventor 黄辉其印建国黄艳
Owner JIANGSU XIXIN VITAMIN
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