Benzotroponoid compounds and preparation method and applications thereof
A technology of pharmaceutical preparations and compounds, applied in the field of benzotropolone analogues and its preparation, can solve problems such as long-term medication, easy rebound, safety concerns and heated discussions
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Embodiment 1
[0046] Example 1 Preparation of compound 1
[0047]
[0048] Take respectively 50 g of epigallocatechin gallate and rutin, dissolve in 10 L of citric acid-sodium hydrogen phosphate buffer (substrate concentration 1%) with a pH of 4.0, add a certain amount of apple polyphenols Oxidase (addition amount is 1.5g / L), oxygen flow rate is 10L / min, stir and react at 80rpm at 25°C for 1.5 hours, after the reaction is over, stop feeding oxygen, and heat to rapidly increase the temperature to 100°C to make the polyphenol Oxidase inactivation, hold for 5 minutes.
[0049] The resulting reaction solution was subjected to polyamide resin column chromatography, the diameter-to-height ratio of the column chromatography was 1:10, the sample volume to column bed volume ratio was 1:4, and the sample loading flow rate was 2 BV / h, followed by water and 5% ethanol aqueous solution , 95% ethanol aqueous solution for elution, collect the eluted part of 95% ethanol, concentrate and dry under reduc...
Embodiment 2
[0054] Example 2 Preparation of Compound 2
[0055]
[0056] Weigh respectively 60 g of epigallocatechin and rutin, dissolve in 10 L of citric acid-disodium hydrogen phosphate buffer (substrate concentration 1.2%) with a pH of 4.5, add a certain amount of blueberry polyphenol oxidase ( The addition amount is 1.5g / L), the ventilation rate is 12L / min, and the reaction is stirred at 80rpm at 25°C for 2 hours. live, hold for 5 minutes.
[0057] The resulting reaction solution was subjected to polyamide resin column chromatography, the diameter-to-height ratio of the column chromatography was 1:10, the ratio of sample volume to column bed volume was 1:4, and the sample loading flow rate was 2 BV / h, followed by water and 5% ethanol aqueous solution , 95% ethanol aqueous solution for elution, collect the eluted part of 95% ethanol, concentrate and dry under reduced pressure at 40°C to obtain a crude extract, use BUCHI medium pressure preparation for further separation and purif...
Embodiment 3
[0059] Example 3 Preparation of compound 3
[0060]
[0061] Weigh 75g each of epigallocatechin gallate and isoquercitrin, dissolve them in 10L of citric acid-sodium hydrogen phosphate buffer (substrate concentration 1.5%) with a pH of 5.0, add a certain amount of apple Polyphenol oxidase (addition amount is 2.0g / L), ventilation rate is 14L / min, under 30 ℃ 120rpm stirring reaction for 2 hours, after the reaction is finished, stop feeding oxygen, heat up the temperature rapidly to 100 ℃ to make polyphenol oxidase Inactivate phenoloxidase by holding for 5 minutes.
[0062] The resulting reaction solution was subjected to polyamide resin column chromatography, the diameter-to-height ratio of the column chromatography was 1:10, the ratio of sample volume to column bed volume was 1:4, and the sample loading flow rate was 2 BV / h, followed by water and 5% ethanol aqueous solution , 95% ethanol aqueous solution for elution, collect the eluted part of 95% ethanol, concentrate and...
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