Method for preparing 7-hydroxymitragynine
A technology of mitragynine and hydroxyl, which is applied in the field of medicine to achieve the effects of low cost, simple reaction operation and high purification yield
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Embodiment 1
[0019] 1) Add 20 mg of mitragynine, 1 mL of tetrahydrofuran and 0.5 mL of water into a 100 mL flask, fill it with argon, then place the flask in a low-temperature reactor and stir; another 32 mg of [bis(trifluoroacetoxy ) Iodo]benzene (PIFA) was dissolved in 1 mL of tetrahydrofuran, then added dropwise into the flask at 0 °C, and reacted for 4 hours;
[0020] 2) Step 1) After the reaction, add 2 mL of saturated sodium bicarbonate solution to adjust the pH of the reaction solution to 8~9, then add 20 mL of ethyl acetate to wash, then extract with saturated saline three times, 15 mL each time, and combine the extractions liquid, then add anhydrous sodium sulfate to dry and filter, and the obtained filtrate is spin-dried to obtain a dark brown crude product;
[0021] 3) Using the ethyl acetate-petroleum ether mixture with a volume ratio of 1:1 as the eluent, the obtained crude product was separated and purified by a basic silica gel column to obtain a light yellow solid with a yi...
Embodiment 2
[0023] 1) Add 20 mg mitragynine, 1 mL tetrahydrofuran and 0.5 mL water into a 100 mL flask, fill with argon, then place the flask in a low-temperature reactor and stir; another 32 mg [bis(trifluoroacetoxy Base) iodo]benzene (PIFA) was dissolved in 1 mL of tetrahydrofuran, then added dropwise into the flask at 0 °C, and reacted for 6 hours;
[0024] 2) Step 1) After the reaction, add 2 mL of saturated sodium bicarbonate solution to adjust the pH of the reaction solution to 8~9, then add 20 mL of ethyl acetate to wash, then extract with saturated saline three times, 15 mL each time, and combine the extractions liquid, then add anhydrous sodium sulfate to dry and filter, and the obtained filtrate is spin-dried to obtain a dark brown crude product;
[0025] 3) Using the ethyl acetate-petroleum ether mixture with a volume ratio of 1:1 as the eluent, the obtained crude product was separated and purified by a basic silica gel column to obtain a light yellow solid with a yield of 65%....
Embodiment 3
[0027] 1) Add 20 mg of mitragynine, 1 mL of tetrahydrofuran and 0.5 mL of water into a 100 mL flask, fill with argon, then place the flask in a low-temperature reactor and stir; another 32 mg of [bis(trifluoroacetoxy ) Iodo]benzene (PIFA) was dissolved in 1 mL of tetrahydrofuran, then added dropwise into the flask at 0 °C, and reacted for 8 hours;
[0028] 2) Step 1) After the reaction, add 2 mL of saturated sodium bicarbonate solution to adjust the pH of the reaction solution to 8~9, then add 20 mL of ethyl acetate to wash, then extract with saturated saline three times, 15 mL each time, and combine the extractions liquid, then add anhydrous sodium sulfate to dry and filter, and the obtained filtrate is spin-dried to obtain a dark brown crude product;
[0029] 3) Using ethyl acetate-petroleum ether mixture with a volume ratio of 1:1 as the eluent, the obtained crude product was separated and purified by basic silica gel column to obtain a light yellow solid with a yield of 70...
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