A kind of benzazepine alkaloid compound and its preparation method and application
A kind of technology of alkaloids and benzodiazepines, which is applied in the field of phytochemistry to achieve the effect of good anti-tobacco mosaic virus activity, good activity and simple structure
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[0025] The preparation method of the benzoheteroquinoline alkaloid compound according to the present invention takes Tang pine grass as a raw material, and is subjected to the steps of extracting extract, silica gel column chromatography and high pressure liquid chromatography separation and purification, and specifically includes:
[0026] A. Extraction of extract: pulverize the whole grass of P. serrata, extract 2~3 times with 95% ethanol reflux, each 35~80min, combine the extracts and concentrate to obtain material a, add tartaric acid solution to dilute in material a to obtain material b, material b is extracted with ethyl acetate for 1~3 times, the water phase is collected to obtain material c, material c is saturated with sodium carbonate, extracted with ethyl acetate again for 1~3 times, the extracted ethyl acetate phases are combined and concentrated under reduced pressure to obtain extract d;
[0027] B, silica gel column chromatography: extract d uses 150-200 mesh si...
Embodiment 1
[0037] Preparation of benzazepine alkaloid compound C 15 H 15 NO 3 , including extract extraction, silica gel column chromatography, high-pressure liquid chromatography separation, the specific steps are as follows:
[0038] (1) Extraction of extract: Take the whole plant of P. serrata, sun-dried, and pulverize to about 35-80 mesh. Weigh 3.0~4.2 kg of the crushed sample, put it in a 50 L glass reactor, add 15~20 L of 95% ethanol, reflux for 35~80 min, and filter out the extract; add 95% to the residue again 15-20 L of ethanol, reflux extraction for 35-80 min, and filter out the extract. The two extracts were combined and concentrated to a small volume, then diluted with 6-10 L of 3% tartaric acid solution, and extracted twice with 6-10 L of ethyl acetate. After the extraction, the aqueous phase was saturated with sodium carbonate, extracted twice with 5-8 L of ethyl acetate again, and the extracted ethyl acetate phases were combined and concentrated under reduced pressure ...
Embodiment 2
[0044] The T. serrata sample was obtained from Heqing County, Dali, Yunnan. Take the whole plant of Tangsong serrata, sun-dried, and crushed to about 40 mesh. Weigh 3.2 kg of the pulverized sample, place it in a 50 L glass reactor, add 16 L of 95% ethanol, reflux for extraction for 38 min, and filter out the extract; add 16 L of 95% ethanol to the residue again, reflux After extraction for 38 min, the extract was filtered off. The two extracts were combined and concentrated to a small volume, then diluted with 8 L of 3% tartaric acid solution, and extracted twice with 8 L of ethyl acetate. After the extraction, the aqueous phase was saturated with sodium carbonate, extracted twice with 6 L of ethyl acetate, and the extracted ethyl acetate phases were combined and concentrated under reduced pressure to obtain 48.2 g of alkaloid fraction extract. After the extract is dissolved in pure methanol, pure ethanol or pure acetone in a weight ratio of 1.5 to 3 times, mix the sample wi...
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