A kind of method utilizing metal reducing agent to prepare matrine from oxymatrine
A technology of oxymatrine and reducing agent, which is applied in the field of natural medicinal chemistry, can solve the problems of no matrine, etc., and achieve the effect of high product purity, low cost and high conversion rate
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Embodiment 1
[0033] Dissolve 100g of pure oxymatrine in water, transfer it to a reaction kettle, add 40g of tin dichloride and 20g of ammonium sulfate, react at 50°C for 4 hours, stop the reaction, concentrate under reduced pressure to a specific gravity of 1.03, and use Toluene extraction; the extract is decompressed and recovered toluene is complete, acetone is added for hot melting, cooling and crystallization, and centrifugation obtains 91.5g of matrine fine-quality goods, and the purity measured by high-efficiency liquid phase normalization method is 99.5%, and oxymatrine is converted into The conversion yield of matrine was 96.9% in terms of moles.
Embodiment 2
[0035] Dissolve 100g of crude oxymatrine (containing 75% oxymatrine) in 50% ethanol, transfer it to a reaction kettle, add 35g metal magnesium, 20g sodium acetate, and react at 80°C for 6 hours, then stop the reaction. Concentrate under reduced pressure to a specific gravity of 1.03, extract with xylene; decompress the extract to recover xylene completely, add acetone to melt, cool and crystallize, and centrifuge to obtain 72.3g of matrine fine product, measured by HPLC normalization method The purity is 98.3%, and the conversion yield of oxymatrine into matrine is 100.9% in terms of moles.
Embodiment 3
[0037] Dissolve 1600g of crude oxymatrine (containing 65% oxymatrine) in water, transfer it to a reaction kettle, add 250g of metallic iron and 500g of sodium chloride, react at 60°C for 8 hours, stop the reaction, and depressurize Concentrate to a specific gravity of 1.03, extract with toluene; depressurize the extract to recover toluene completely, add acetone to melt, cool and crystallize, and centrifuge to obtain 992.5g of matrine fine product, the purity measured by HPLC normalization method is 99.0% , the conversion yield of oxymatrine into matrine was 100.6% in moles.
[0038] The resulting product was analyzed by high-performance liquid chromatography (HPLC). The HPLC chromatographic conditions were: using octadecyl bonded phase silica gel as the stationary phase, methanol-0.2% phosphoric acid solution (10:90, V / V) as the mobile phase, The flow rate is 1 mL / min, the detection wavelength is 205 nm, and the column temperature is 25-50°C.
[0039] figure 1 It is a high-...
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