Bromodihydroartemisinin and preparation method thereof
A dihydroartemisinin, brominated technology, applied in the field of chemistry, can solve the problems of limited application, toxic and side effects of chemical drugs, large toxic and side effects, etc.
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Embodiment 1
[0022] Mix 9g of dihydroartemisinin and 300ml of acetonitrile, and introduce 2ml of bromine water at a temperature of 40°C. The bromine water conduit should go deep into the bottom of the reactant while stirring so that the reactant can fully contact with bromine water. After 50 minutes, pour into Add 9ml of 10% sodium thiosulfate solution to the reaction mixture, collect the organic phase, then add 60ml of 10% sodium bicarbonate solution, add ethyl acetate to collect the organic layer, and dehydrate the organic layer with anhydrous sodium sulfate and concentrate under reduced pressure to obtain Crystallized and dried to obtain brominated dihydroartemisinin as yellowish block crystals, which were recrystallized with n-hexane to obtain white needle crystals.
[0023] IRv KBr max : 1745, 1115, 831, 881cm -1 . The infrared spectrum of brominated dihydroartemisinin is shown in Figure 3. Compared with the infrared spectrum of dihydroartemisinin, there are more bromine peaks such...
Embodiment 2
[0114] 1.5g of dihydroartemisinin and 50ml of dimethylformamide were mixed, and 0.3ml of bromine was introduced at 25°C. After 5 minutes, 15ml of 10% sodium thiosulfate solution was added to the reaction mixture, and the organic phase was collected. Then add 30ml of 10% sodium bicarbonate solution, add ethyl acetate to collect the organic layer, dehydrate the organic layer with anhydrous sodium sulfate and concentrate under reduced pressure to form crystals, wash the crystals with n-hexane, filter the crystals, and dry to obtain bromobis Hydrogenartemisinin is yellowish block crystal. Recrystallization with n-hexane gave white needle crystals.
Embodiment 3
[0116] Mix 1.5g of dihydroartemisinin and 50ml of acetic acid, add 0.3ml of bromine water at 0°C, stir and react for 200 minutes, add water and stir for debromination, collect the organic layer and concentrate under reduced pressure to form crystals, wash the crystals with n-hexane , filtered out the crystals, and dried to obtain brominated dihydroartemisinin. After drying, white needle-like crystals were obtained.
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