Chroman compound, as well as preparation method and application thereof
A compound and chroman technology, applied in the field of chroman compounds and their preparation, can solve the problems such as few reports of the turtle worm, and achieve the effects of extensive pharmacological activity, easy operation and high product purity
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Embodiment 1
[0040] Embodiment 1 The preparation of chroman compound
[0041] Take 10kg ground soft-shelled turtle, extract it with 10L methanol for 2 weeks, suspend the methanol extract with 1L distilled water after concentration, extract the water suspension with 1L ethyl acetate for 3 times, and concentrate the ethyl acetate extract to obtain 23g extract ; Mix the sample with silica gel (100 mesh, 100g), and perform normal phase silica gel column chromatography (200-300 mesh, 1kg; silica gel column size L500mm, 120mm), followed by gradient elution with volume ratio 9:1, 5:1, 3:1, 1:1, 1:3, 1:9 petroleum ether / ethyl acetate mixture, each gradient elution 5L ; Fractions were detected by TLC, the fractions with an elution ratio of 5:1 were collected, combined, concentrated, and then recrystallized with acetone (at room temperature) to obtain the target compound.
Embodiment 2
[0042] Embodiment 2 The preparation of chroman compound
[0043] Take 10kg ground soft-shelled turtle, extract with 5L of ethanol under reflux, suspend the ethanol extract with 1L of distilled water after concentration, extract the water suspension with 1L of chloroform for 3 times, and obtain 234g of extract after concentration of the chloroform extract; use silica gel (100 mesh, 100g) for normal phase silica gel column chromatography (200-300 mesh, 1kg; silica gel column size L500mm, 120mm), followed by gradient elution with volume ratio 9:1, 5:1, 3:1, 1:1, 1:3, 1:9 petroleum ether / ethyl acetate mixture, each gradient elution 5L ; Fractions were detected by TLC, the fractions with an elution ratio of 5:1 were collected, combined, concentrated, and then recrystallized with acetone (at room temperature) to obtain the target compound.
Embodiment 3
[0044] Embodiment 3 preparation of chroman compound
[0045] Take 10kg of pulverized ground beetles, extract with 5L of methanol / ethanol mixture, concentrate the methanol / ethanol extract to obtain 366g of extract, mix the sample with 100g of diatomaceous earth, soak in 5L of chloroform for 3 times, and carry out normal phase silica gel column layer Analysis (200-300 mesh, 1kg; silica gel column size L500mm, 120mm), followed by gradient elution with volume ratio 9:1, 5:1, 3:1, 1:1, 1:3, 1:9 petroleum ether / ethyl acetate mixture, each gradient elution 5L ; Fractions were detected by TLC, the fractions with an elution ratio of 5:1 were collected, combined, concentrated, and then recrystallized (at room temperature) with acetone / n-hexane (volume ratio 1:1) to obtain the target compound.
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