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

A technology of lupus B, high purity, applied in the direction of organic chemistry, etc., can solve the problems of low yield of lupus B, complicated extraction and purification process operations, etc., and achieves reduced extraction and purification costs, good elution effect, and reduced The effect of impurity content

Active Publication Date: 2014-08-06
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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PUM

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Abstract

The invention discloses a method for preparing high-purity wolfbane B, which comprises the following steps: pulverizing Euphorbia chamaejasma, extracting with ethanol reflux, filtering the extract to obtain a filtrate; concentrating the filtrate, recovering ethanol to obtain a thick paste; Add 5 to 10 times the amount of silica gel to the thick paste, mix well, dry, perform column chromatography with silica gel as the carrier, elute with the eluent and collect the eluent; concentrate the eluent, recover the solvent, and obtain Coarse crystals of chamaejamabolin; dissolve the crude crystals with ethanol, add silica gel to mix, dry, and perform silica gel column chromatography for 2 to 3 times to obtain pure chamaejamacin. The extraction and purification cost of the method of the invention can be reduced by about 20%, and at the same time, the energy consumption can be greatly reduced, and the extraction efficiency of chamaejasme B can be increased to more than 30%. The prepared chamaejamasin B has a purity of more than 99%, and is especially suitable as a standard substance for content determination of chamaemachamata medicinal material and related preparation Jiejieling tablets.

Description

Technical field [0001] The invention involves the extraction and purification method of a compound, which specializes in a method for preparing a high -purity wolf poison. Background technique [0002] Wolf toxic is one of the main anti -tuberculosis components in wolf toxic medicinal materials, which is easily soluble in alcohol and slightly soluble in the water. [0003] As a chemical control product of wolf poisoning medicinal materials, the purity of wolf poison Bin directly affects the accuracy and reliability of drug quality control.The conventional wolf poison ethyl element extraction and purification operation generally breaks the wolf poison eurites first, then boiled in water, filter the boiled liquid, concentrate, and then perform alcohol -lift and silicone column layer.This method adopted in the "Research on the Research of the Wolf Poison Euphorbia Chemical Products" reported by He Nansheng and others. The public method is: take the wolf poison eurites with water and...

Claims

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Application Information

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Patent Type & Authority Patents(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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