Pheophorbide curcumin ester with photosensitive activity and preparation method and application thereof
A technology of pheophorbide and curcumin ester, which is applied in the field of pheophorbide and curcumin ester and its preparation, can solve the problems of weak tissue penetration and weak tumor killing effect, and achieve deep tissue penetration , It is convenient for industrial production and the reaction conditions are easy to control
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Embodiment 1
[0021] Pheophorbide (0.6g, about 1mmol) and curcumin (0.4g, about 1mmol), add 50ml of chloroform, stir to dissolve; add N,N-dicyclohexylcarbodiimide DCC (0.1g , about 0.5mmol) to react, then slowly add DMAP (0.05g about 0.5mmol) to catalyze the reaction, and react at 30°C for 4 hours. After the reaction was completed, the mixed solution was washed three times with 100 ml of water, and the organic phase was dried over anhydrous magnesium sulfate, filtered, and distilled under reduced pressure to obtain 0.8 g of the product.
[0022] The product was analyzed by element composition, containing C70.3%, H5.8%, O17.7%, N6.2%, molecular weight 905, molecular formula: C 53 h 52 N 4 o 10 , NMR confirmed that there are 3 methoxyl hydrogens, 1 hydroxyl hydrogen, 5 carbonyl carbons, 2 benzene ring structures and 1 porphyrin structure in its structure, so it is deduced that its structure is 1 molecule of pheophorbide and turmeric The ester of element formation, as the structure of form...
Embodiment 2
[0026] Pheophorbide (0.6g, about 1mmol) and curcumin (0.4g, about 1mmol), add 50ml ethyl acetate, stir and dissolve; add N,N-dicyclohexylcarbodiimide DCC ( 0.2g, about 1mmol) to react, then slowly add DMAP (0.1g about 1mmol) to catalyze the reaction, and react at 40°C for 6 hours. After the reaction was completed, the mixture was washed three times with 100 ml of saturated brine, and the organic phase was dried over anhydrous sodium sulfate, filtered, and distilled under reduced pressure to obtain 0.9 g of the product.
[0027] The product was analyzed by element composition, containing C69.8%, H5.8%, O18.6%, N5.9%, molecular weight 947, molecular formula: C 55 h 54 N 4 o 11 , NMR confirmed that there are 3 methoxy hydrogens, 6 carbonyl carbons, 2 benzene ring structures and 1 porphyrin structure in its structure. Compared with formula III, there is one hydroxyl hydrogen less and one more acetyl group, so it is deduced that its The structure is that of formula IV.
[0028...
Embodiment 3
[0031] Pheophorbide (2.8g, about 5mmol) and curcumin (0.4g, about 1mmol), add 50ml of benzene, stir to dissolve; add concentrated sulfuric acid (0.5g, about 5mmol) dropwise under nitrogen protection, and react at 60°C for 8 Hours. After the reaction was completed, the mixture was washed three times with 100 ml of saturated brine, and the organic phase was dried over anhydrous sodium sulfate, filtered, and distilled under reduced pressure to obtain 1.5 g of the product.
[0032] The product was analyzed by element composition, containing C70.8%, H5.9%, O15.5%, N7.8%, molecular weight 1442, molecular formula: C 85 h 84 N 8 o 14 , NMR confirmed that there are 4 methoxy hydrogens, 8 carbonyl carbons, 2 benzene ring structures and 2 porphyrin structures in its structure, so it is speculated that its structure is formed by 2 molecules of pheophorbide and 1 molecule of curcumin Esters, such as the structure of formula II.
[0033] The product is insoluble in water, but soluble i...
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