Benzoporphyrin chlorophyll photosensitizer and its preparation process and use
A technology of benzochloroporphyrin and chloroporphyrin, applied in the field of medicine, can solve the problems of high phototoxicity and complexity of normal tissues, and low photodynamic effect of target lesions
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Embodiment 1
[0057] Example 1 Chlorin f dimethyl ester (V 1 ) preparation
[0058]Take chlorin f(VI 1 ) 0.65g (1.21mmol) was dissolved in 50mL redistilled tetrahydrofuran (THF), and 10mL (6.67mmol) of freshly prepared 2.8% (w / v) diazomethane ether solution was added at 0°C to react 10mM, and then add 0.2mL Decompose excess diazomethane with glacial acetic acid, recover 2 / 3 of THF under reduced pressure, dilute with 50mL chloroform, wash with water until neutral, dry over anhydrous sodium sulfate, recover solvent, and separate by silica gel H column chromatography after drying to obtain black powder V 1 0.45g, melting point 211-212°C, yield 66.2%. UV lambda max (CH 2 Cl 2 ) nm: 666 (7.1×10 4 ), 610 (7.3×10 3 ), 529 (6.2×10 3 ), 499 (1.7×10 4 ), 401 (1.9×10 5 ) (soret). 1 H NMR (500Hz, CDCl 3 )δ ppm: 9.82, 9.77, 9.63 and 8.75 (each s, each 1H, 4 × meso-H), 8.07 (dd, 1H, J = 17.9 and 11.5Hz, 2a-H x ), 6.33 (d, 1H, J=17.9Hz, 2b-H B ), 6.15 (d, 1H, J=11.5Hz, 2b-H A ), 4.50(m, 2H,...
Embodiment 2
[0059] Example 2 Chlorin p 6 Trimethyl ester (V 2 ) preparation
[0060] 2.0g of purpurin-18 (3.55mmol) was dissolved in 50mL of tetrahydrofuran, 200mL of methanol and 250mL of 20% (w / v) sodium hydroxide aqueous solution were added, and the reaction was stirred at room temperature until the ultraviolet absorption peak at 698nm disappeared, which took about 1h. Then it was diluted with 500 mL of water, neutralized with 10% (w / v) sulfuric acid to pH 5-6, extracted with diethyl ether (200 mL×3), and dried over anhydrous sodium sulfate. Add 30mL (20mmol) of 2.8% (w / v) diazomethane ether solution to the ether solution under ice-salt bath cooling, react for 10mM, then add 0.5mL glacial acetic acid to decompose the excess diazomethane, recover the solvent, dry it through silica gel H Column chromatography separated black powder V 2 1.8g, melting point 232-233°C, yield 81.3%. UV lambda max (CH 2 Cl 2 ) nm: 669 (6.3×10 4 ), 615 (8.2×10 3 ), 530 (9.8×10 3 ), 499 (1.7×10 4 ), ...
Embodiment 3
[0061] Example 3 Chlorin e 6 Trimethyl ester (V 3 ) preparation
[0062] According to the method of embodiment 1, 3.6g (6.04mmol) chlorin e 6 (VI 3 ) reacted with 2.8% (w / v) diazomethane ether solution 40mL (26.67mmol) to obtain a black solid V 3 2.43g, melting point 209-210°C, yield 63.1%. UV lambda max (CH 2 Cl 2 ) nm: 664 (1.3×10 5 ), 608 (1.5×10 4 ), 530 (1.5×10 4 ), 501 (3.8×10 4 ), 402 (3.7×10 5 ) (soret). 1 H NMR (500Hz, CDCl 3 )δ ppm: 9.69, 9.56 and 8.75 (each s, each 1H, 3×meso-H), 8.05 (dd, 1H, J=17.8 and 11.5Hz, 2a-H x ), 6.34 (d, 1H, J=17.8Hz, 2b-H B ), 6.13 (d, 1H, J=11.5Hz, 2b-H A ), 5.34 (d, 1H, J=18.9Hz, 10-H A ), 5.23 (d, 1H, J=18.9Hz, 10-H B ), 4.42(m, 2H, 7, 8-H), 4.25, 3.76, 3.61, 3.57, 3.46 and 3.29(each s, each 3H, 5-, 1-, 3-Me and OMe×3), 3.79( q, 2H, J=7.5Hz, 4a-CH 2 ), 2.54 (m, 2H, 7b-CH 2 ), 2.18 (m, 2H, 7a-CH 2 ), 1.75 (d, 3H, J = 7.0Hz, 8-Me), 1.70 (t, 3H, J = 7.5Hz, 4b-Me), -1.28and-1.46 (each br s, each 1H, NH in the ring ×2...
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