Method for preparing diosgenin through microwave-assisted acidic ionic liquid catalysis
An acidic ionic liquid, diosgenin technology, applied in organic chemistry, steroids, etc., can solve the problems of large discharge, time-consuming biotransformation and enzymatic methods, complicated production processes, etc. Stable, shortened response time effect
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Embodiment 1
[0013] Take 100 g of dry powder of Dioscorea Zingiberensis C.H.Wright, add 50% ethanol by volume according to the ratio of solid to liquid (1:10 (g / mL)) and reflux extract for 3 times, each time for 1 hour. After extraction, centrifuge and take the supernatant. The supernatants were combined, and the ethanol was recovered to obtain a saponin-containing aqueous solution. After the aqueous solution was extracted twice with saturated n-butanol at a ratio of 1:1 (V:V), the n-butanol fractions were combined. Recover n-butanol under reduced pressure to dryness to obtain total saponins. Dilute the acidic ionic liquid with deionized water to prepare a 2mol / L ionic liquid solution. According to the ratio of solid to liquid 1:10 (g / mL), it is mixed with saponin and added to the microwave reaction tank. The reaction temperature was set at 80° C., and after reacting under microwave for 20 min, the reaction solution was cooled to room temperature and filtered. The filtrate was rotary e...
Embodiment 2
[0015] Take 200 g of dry powder of Dioscorea Zingiberensis C.H.Wright, add 70% ethanol by volume according to the ratio of solid to liquid (1:15 (g / mL)) and reflux extract twice, each time for 2 hours. After extraction, centrifuge and take the supernatant. The supernatants were combined, and the ethanol was recovered to obtain a saponin-containing aqueous solution. After the aqueous solution was extracted twice with saturated n-butanol at a ratio of 1:1 (V:V), the n-butanol fractions were combined. Recover n-butanol under reduced pressure to dryness to obtain total saponins. Dilute the acidic ionic liquid with deionized water to prepare a 4mol / L ionic liquid solution. According to the ratio of solid to liquid 1:10 (g / mL), it is mixed with saponin and added to the microwave reaction tank. The reaction temperature was set at 100° C., and after reacting under microwave for 15 minutes, the reaction liquid was cooled to room temperature and filtered. The filtrate was rotary eva...
Embodiment 3
[0017] Take 300 g of dry powder of Dioscorea Zingiberensis C.H.Wright, add 80% ethanol at a volume ratio according to the ratio of solid to liquid (1:20 (g / mL)) and reflux extract twice, each time for 1 hour. After extraction, centrifuge and take the supernatant. The supernatants were combined, and the ethanol was recovered to obtain a saponin-containing aqueous solution. After the aqueous solution was extracted twice with saturated n-butanol at a ratio of 1:1 (V:V), the n-butanol fractions were combined. Recover n-butanol under reduced pressure to dryness to obtain total saponins. Dilute the acidic ionic liquid with deionized water to prepare a 6mol / L ionic liquid solution. According to the ratio of solid to liquid 1:20 (g / mL), it is mixed with saponin and added to the microwave reaction tank. The reaction temperature was set at 110° C., and after reacting under microwave for 10 min, the reaction solution was cooled to room temperature and filtered. The filtrate was rotar...
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