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Method for preparing 2,4-dihydroxy-6-methoxy-3-methylacetophenone with high purity

A lupus B, high-purity technology, applied in the direction of organic chemistry, can solve the problems of complicated extraction and purification process, low yield of lupus The effect of impurity content

Active Publication Date: 2012-10-03
广东恒健制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction and purification process of this method is complicated to operate, and the yield of chamaejasme B is also low, so it is necessary to improve the existing method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A method for preparing high-purity wolfbane B, comprising the steps of:

[0027] 1) Crush Euphorbia chamaejasma into a 20-mesh coarse powder, reflux extract with 13 times the amount of 70% (v / v) ethanol for 3 times, each time for 2 hours, combine the extracts and filter to obtain the filtrate;

[0028] 2) Concentrating the filtrate, reclaiming ethanol, obtaining a thick paste with a density of 1.15 g / ml;

[0029] 3) Add 7 times the mass of silica gel to the thick paste, mix well, dry at 60°C, perform column chromatography with silica gel as the carrier, elute with eluent and collect the eluent, the eluent is petroleum ether: acetic acid Ethyl ester=10:4 (v / v) mixture;

[0030] 4) Concentrating the collected eluent, recovering the solvent, and obtaining crude crystals of chamaejasme B;

[0031] 5) Dissolve the crude crystals in ethanol with 7 times the mass concentration of 70% (v / v), add 7 times the mass of silica gel, dry at 60°C, and then use the same eluent to perf...

Embodiment 2

[0034] A method for preparing high-purity wolfbane B, comprising the steps of:

[0035] 1) Crush Euphorbia chamaejasma into a 20-mesh coarse powder, reflux extract with 10 times the amount of 80% (v / v) ethanol for 3 times, each time for 2 hours, combine the extracts and filter to obtain the filtrate;

[0036] 2) Concentrating the filtrate, reclaiming ethanol, obtaining a thick paste with a density of 1.20 g / ml;

[0037] 3) Add 10 times the mass of silica gel to the thick paste, mix well, dry at 60°C, perform column chromatography with silica gel as the carrier, elute with eluent and collect the eluent, the eluent is petroleum ether: acetic acid Ethyl ester=10:4 (v / v) mixture;

[0038] 4) Concentrating the collected eluent, recovering the solvent, and obtaining crude crystals of chamaejasme B;

[0039] 5) Dissolve the crude crystals in ethanol with 5 times the mass concentration of 70% (v / v), add 10 times the mass of silica gel, dry at 60°C, and then perform silica gel column...

Embodiment 3

[0042] A method for preparing high-purity wolfbane B, comprising the steps of:

[0043] 1) Crush Euphorbia chamaejasma into 20-mesh coarse powder, reflux extract with 15 times the amount of 60% (v / v) ethanol for 3 times, each time for 2 hours, combine the extracts and filter to obtain the filtrate;

[0044] 2) Concentrating the filtrate, reclaiming ethanol, obtaining a thick paste with a density of 1.13 g / ml;

[0045] 3) Add 5 times the mass of silica gel to the thick paste, mix well, dry at 60°C, perform column chromatography with silica gel as the carrier, elute with eluent and collect the eluent, the eluent is petroleum ether: acetic acid Ethyl ester=10:4 (v / v) mixture;

[0046] 4) Concentrating the collected eluent, recovering the solvent, and obtaining crude crystals of chamaejasme B;

[0047] 5) Dissolve the crude crystals in ethanol with 5 times the mass concentration of 70% (v / v), add 5 times the mass of silica gel, dry at 60°C, and then use the same eluent to perfor...

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Abstract

The invention discloses a method for preparing 2,4-dihydroxy-6-methoxy-3-methylacetophenone with high purity. The method comprises the following steps: Euphorbia fischeriana is grinded and subjected to reflux extraction by using ethanol, then extract is filtrated to obtain a filtrate; the filtrate is condensed for recycling ethanol to obtain a thick paste; silica gel is added into the paste with a ratio of 5-10:1 of the silica gel to the paste to obtain a mixture, then the mixture is blended homogeneously, dried, subjected to column chromatography by using the silica gel as a carrier and eluted with an eluent, and the eluent is collected; the eluent is condensed to recycle solvents to obtain crude crystal of 2,4-dihydroxy-6-methoxy-3-methylacetophenone; the crude crystal is dissolved into ethanol, then silica gel is added and mixed to obtain another mixture, then the mixture is dried and subjected to column chromatography by using silica gel for 2-3 times to obtain pure 2,4-dihydroxy-6-methoxy-3-methylacetophenone. Extraction and purification costs of the method provided by the invention can be reduced by about 20%, at the same time, energy consumption can be significantly reduced and extraction efficiency can be increased to over 30%. The prepared 2,4-dihydroxy-6-methoxy-3-methylacetophenone has a purity of more than 99% and is especially suitable to be used as a standard substance for measuring contents of Stellera chamaejasme medical materials and related preparations like JIEHELING tablets.

Description

technical field [0001] The invention relates to a method for extracting and purifying a compound, in particular to a method for preparing high-purity chamaejasme B. Background technique [0002] Chamaejasma B is one of the main anti-tuberculosis ingredients in chamaejasma, easily soluble in alcohol and slightly soluble in water. [0003] As a chemical reference substance of chamaejasma, the purity of chamaejamas directly affects the accuracy and reliability of drug quality control. Conventional extraction and purification of Euphorbia chamaejasmin is generally performed by crushing Euphorbia chamaejasma first, then boiling in water, filtering and concentrating the boiling liquid, and then carrying out alcohol extraction and silica gel column chromatography. This method was adopted in the "Research on Chemical Reference Substances of Euphorbia chamaejasma" reported by He Nansheng et al. The disclosed method is as follows: take Euphorbia chamaejasma and add water to cook twic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/32C07D311/40
Inventor 冯淡开黄聪燕江志华康丽红钟慧敏黄奇建
Owner 广东恒健制药有限公司
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