Preparation method and application of 9-position substituted bifunctional berberine derivatives
A technology of berberine and derivatives, applied in the field of food and pharmaceuticals, can solve the problems of malabsorption, affecting systemic therapeutic effect, and low oral bioavailability
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Embodiment 1
[0021] a) Synthesis of Berberine
[0022] Add 7.4g of berberine to a 250mL round flask, heat at 190-200°C for about 30min at a vacuum of 20-30mmHg, the yellow solid gradually turns dark red, cool to room temperature in a vacuum desiccator, and purify by silica gel column chromatography. Obtained 4.7 g of dark red powder with a yield of 75%.
[0023] b) Synthesis of 9-O-3-bromo-ethyl berberine hydrobromide
[0024] Add 3.2g (10mmol) of berberine into a 25mL round bottom flask, add 30mL of DMF to dissolve, heat at 70°C, add 3.5g (20mmol) of 1,2-bromoethane, follow the reaction by TLC, add 100mL of anhydrous Diethyl ether, precipitated solid, filtered, and purified by silica gel column chromatography to obtain 3.9 g of 9-O-3-bromo-ethyl berberine hydrobromide, yield 76%
[0025] c) Synthesis of fluvastatin-9-O-acetate berberine hydrobromide
[0026] Add 411 mg (1 mmol) fluvastatin to a 25 mL round bottom flask, add 5 mL DMF to dissolve, stir at room temperature, add 44 g (1.1 ...
Embodiment 2
[0028] a) Synthesis of Berberine
[0029] Same as a) in Example 1
[0030] b) Synthesis of 9-O-3-hydroxyl-ethyl berberine hydrobromide
[0031] Same as b) in Example 1
[0032] c) Synthesis of simvastatin-9-O-acetate berberine hydrobromide
[0033] Add 437 mg (1 mmol) of simvastatin to a 25 mL round bottom flask, add 5 mL of DMF to dissolve, stir at room temperature, add 44 g (1.1 mmol) of sodium hydroxide, stir for 10 min, then add 9-O-3-bromo-ethyl berberine 509 mg (1 mmol) of hydrobromide, heated to 70°C, stirred for reaction, followed by TLC, after the reaction was complete, 20 ml of anhydrous ether was added, and solid was precipitated, filtered to obtain simvastatin-9-O-acetate berberine Hydrobromide 746mg, yield 86%. ESI-MS(M+H) + m / z calcd C 45 h 56 NO 10 + for 771.39 found 771.40.
Embodiment 3
[0035] a) Synthesis of Berberine
[0036] Same as a) in Example 1
[0037] b) Synthesis of 9-O-3-hydroxyl-ethyl berberine hydrobromide
[0038] Same as b) in Example 1
[0039] c) Synthesis of pitavastatin-9-O-acetate berberine hydrobromide
[0040] Add 420 mg (1 mmol) of pitavastatin to a 25 mL round bottom flask, add 5 mL of DMF to dissolve, stir at room temperature, add 44 g (1.1 mmol) of sodium hydroxide, stir for 10 min, then add 9-O-3-bromo-ethyl berberine 509 mg (1 mmol) of hydrobromide, heated to 70°C, stirred and reacted, TLC followed the reaction, after the reaction was complete, 20 ml of anhydrous ether was added to precipitate a solid, filtered to obtain pitavastatin-9-O-acetate berberine Hydrobromide 709mg, yield 84%. ESI-MS(M+H) + m / z calcd C 46 h 41 FNO 8 + for755.28found755.28.
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