Preparation method of cynandione A
A technology of uranone and Baishouwu, which is applied in the field of natural medicinal chemistry, can solve the problems of cumbersome method of diketone A, complex components of Baishouwu, and difficulty in industrialized production, etc., and achieves simple and feasible method, easy industrial production, The effect of less impurity dissolution
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Embodiment 1
[0018] Dry and pulverize Baishouwu to 80 meshes, take 2kg and put it into a supercritical extraction kettle, set the extraction pressure to 20MPa, the temperature to 40°C, and feed liquid CO2 at 20kg / h. After the above parameters are reached, feed 90% ethanol solution at 2kg / h to make Entrainer, dynamic extraction for 3 hours, analyze the extract under the conditions of pressure 6MPa and temperature 50°C, add 100g of polyamide resin to the obtained extract to dry, crush the dried product and pack it into a column, take 500ml of 60% ethanol solution to precipitate impurities, and then take 400ml of 90% ethanol Precipitate the target component, concentrate the eluent under reduced pressure to about 50ml, transfer it to a separatory funnel, add an equal volume of chloroform for extraction 3 times, concentrate the extract to about 30ml, place the crystals, filter out the crystals, reflow with absolute ethanol to dissolve the recrystallization, and dry The light yellow crystal radix...
Embodiment 2
[0020] Dry and pulverize Baishouwu to 40 meshes, take 4kg and put it into a supercritical extraction kettle, set the extraction pressure to 30MPa, the temperature to 45°C, and feed liquid CO2 at 25kg / h. After reaching the above parameters, feed 99% methanol solution at 4kg / h to make Entrainer, dynamic extraction for 3 hours, analyze the extract under the conditions of pressure 7MPa and temperature 60°C, add 200g of polyamide resin to the obtained extract to dry, crush the dried product and pack it into a column, take 1200ml of 50% ethanol solution to remove impurities, and then take 1200ml of 80% ethanol Elute the target component, concentrate the eluent under reduced pressure to about 150ml, transfer it to a separatory funnel, add an equal volume of chloroform for extraction twice, concentrate the extract to about 80ml, place the crystals, filter out the crystals, and then reflux with absolute ethanol to dissolve and recrystallize. Dried to obtain pale yellow crystal diketone ...
Embodiment 3
[0022] Dry and pulverize Baishouwu to 60 meshes, take 4kg and put it into a supercritical extraction kettle, set the extraction pressure to 25MPa, the temperature to 50°C, and feed liquid CO2 at 20kg / h. After reaching the above parameters, feed anhydrous acetone solution at 3kg / h for Entrainer, dynamic extraction for 3 hours, analyze the extract under the conditions of pressure 10MPa and temperature 50°C, add 200g of polyamide resin to the obtained extract to dry, crush the dried product into a column, take 1000ml of 60% ethanol solution to remove impurities, and then take 600ml of 99% ethanol Precipitate the target component, concentrate the eluent under reduced pressure to about 120ml, transfer it to a separatory funnel, add an equal volume of chloroform for extraction 3 times, concentrate the extract to about 70ml, place the crystals, filter the crystals, reflow with absolute ethanol to dissolve the recrystallization, and dry The light yellow crystal radix diketone A was obt...
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