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
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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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