Preparation method of ailanthinone
A technology of Ailanthus ketone and Ailanthus ailanthus, which is applied in the field of preparation of Ailanthus ketone extracted from plants, achieves the effects of less pollution, less energy consumption, and is conducive to large-scale production operations
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Embodiment 1
[0018] Take 10Kg of fresh bark of Ailanthus sinensis, add 5 times its mass and volume of ammonia solution with pH=9, soak for 24 hours, filter, adjust the pH of the filtrate to neutral with hydrochloric acid, concentrate, and pass the concentrated solution through AB-8 macroporous adsorption resin Column adsorption, water elution to remove impurities, 60% ethanol elution, collect 3 times the column volume eluate, recover ethanol under reduced pressure to the end, refrigerate for 12 hours to crystallize, filter, take the filter residue, add acetone for recrystallization, wash, After drying, 1.23 g of Ailanthione was obtained, and the purity was 98.2% as detected by HPLC.
Embodiment 2
[0020] Take 10Kg of fresh bark of Ailanthus sinensis, add 10 times its mass and volume of pH=13 KOH aqueous solution, soak for 72 hours, filter, adjust the pH of the filtrate to neutral with hydrochloric acid, concentrate, and pass the concentrated solution through AB-8 macroporous adsorption resin column Adsorption, water elution to remove impurities, 85% ethanol elution, collect 8 times the column volume eluate, recover ethanol under reduced pressure to the end, refrigerate for 36 hours to crystallize, filter, take the filter residue, add acetone for recrystallization, wash and dry That is, 1.62 g of Ailanthonone was obtained, and the purity was 97.4% as detected by HPLC.
Embodiment 3
[0022] Take 10Kg of fresh bark of Ailanthus sinensis, add 8 times its mass and volume of NaOH aqueous solution with pH=10, soak for 36 hours, filter, adjust the pH of the filtrate to neutral with hydrochloric acid, concentrate, and pass the concentrated solution through AB-8 macroporous adsorption resin column Adsorption, water elution to remove impurities, 80% ethanol elution, collect 5 times the column volume eluate, recover ethanol under reduced pressure to the end, refrigerate for 24 hours to crystallize, filter, take the filter residue, add acetone for recrystallization, wash and dry That is, 1.54 g of Ailanthus ketone was obtained, and the purity was 98.8% as detected by HPLC.
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