Synthesis method of novel gossypol derivative
A synthesis method and a derivative technology are applied in the synthesis field of a novel gossypol derivative Desapogossypolone to achieve the effects of saving time, reducing synthesis cost and synthesis time, and improving synthesis efficiency and yield.
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Embodiment 1
[0027] Weigh 5 grams of gossypol acetate with a balance, add 15 ml of 20% sodium hydroxide, and stir and react at 40°C for 300 minutes. After the reaction is completed, cool and add 15 ml of 75% concentrated sulfuric acid. Extract with diethyl ether two to three times, and concentrate to dryness in vacuo to obtain about 4.8 g of the initial product I, which is gray-green in color. Dissolve the initial product I with 9.6ml of dioxane, add 4.8ml of acetic anhydride, stir the reaction at 50°C for 120 minutes, cool to room temperature and extract 2-3 times with ethyl acetate, concentrate to dryness under vacuum, and use acetic acid Ethyl ester was recrystallized and purified to obtain 3.6 g of pure product II, which was pale yellow in color. Weigh 3.6g of the product II, add 18ml of concentrated sulfuric acid to remove isopropyl reagent, react at 80°C for 120 minutes, cool to room temperature and extract 2-3 times with ether, concentrate to dryness under vacuum, and recrystallize ...
Embodiment 2
[0029] Weigh 5 grams of gossypol acetate with a balance, add 50 ml of 30% sodium hydroxide, and stir and react at 90°C for 30 minutes. After the reaction is completed, cool and add 1 ml of 98% concentrated sulfuric acid. Extracted two to three times with ethyl acetate, and concentrated to dryness in vacuo to obtain about 4.8 g of the initial product I, which was gray-green in color. Dissolve the initial product I with 48ml of dioxane, add 48ml of glacial acetic acid, stir and react at 200°C for 20 minutes, cool to room temperature and extract with acetone 2-3 times after completion, concentrate to dryness under vacuum, and reconstitute with chloroform Purification by crystallization can obtain 3.6 g of pure product II, which is pale yellow in color. Weigh 3.6g of product II, add 36ml of concentrated sulfuric acid to remove isopropyl reagent, react at 10°C for 10 minutes, cool to room temperature and extract with ethanol 2-3 times after completion, concentrate to dryness under ...
Embodiment 3
[0031] Weigh 5 grams of gossypol acetate with a balance, add 50 ml of 45% sodium hydroxide, stir and react at 120°C for 30 minutes, after the reaction is completed, place the reactor in ice water, and add 1 ml of 98% concentrated sulfuric acid. Extracted two to three times with petroleum ether, and concentrated to dryness in vacuo to obtain about 4.8 g of the initial product I, which was gray-green in color. Dissolve the initial product I with 48ml of dioxane, add 24ml of acetic anhydride, stir the reaction at 200°C for 20 minutes, cool to room temperature after the end and let it stand for 120 minutes, extract 2-3 times with ethanol, concentrate to dryness under vacuum, use Ethyl acetate was recrystallized and purified to obtain 3.6 g of pure product II, which was pale yellow in color. Weigh 3.6g of product II, add 36ml of concentrated sulfuric acid to remove isopropyl reagent, react at 10°C for 10 minutes, cool to room temperature and extract with ethanol 2-3 times after com...
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