8-dihalo methylene dihydroberberine compound and anti-infection and anti-inflammatory application thereof
A technology of dihalomethylene dihydroberberine and compound is applied in the application field of preparing anti-microbial infection and anti-inflammatory products, and can solve the problems of structural change, chemical structure instability, influence on pharmacological action and the like
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experiment example (1
[0046] Experimental example (1) Preparation process and structure identification data of compound 1
[0047] Coptisine hydrochloride (2.0g, 5.62mmol) was dissolved in 200mL of chloroform-methanol (3:1) mixed solvent in the reaction flask, 24ml of concentrated ammonia was added, stirred and reacted at room temperature for 24h, then the chloroform layer was separated, and The chloroform layer was washed twice with water and washed with anhydrous MgSO 4 After drying, it was filtered; the filtrate was evaporated to dryness, and the resulting crude product was purified by silica gel column chromatography, eluting with dichloromethane, and the eluate was concentrated to obtain 617 mg of 8-trichloromethyldihydrocoptisine as a light yellow solid, with a yield of 25.0%. 1 H NMR (500MHz, CDCl 3 )δ:2.63–2.78(m,1H,NCH 2 C H 2 ),3.35(m,1H,NCH 2 C H 2 ),3.71(m,1H,NC H 2 CH 2 ),3.78-3.90(m,1H,NC H 2 CH 2 ),5.42(s,1H,CH-CCl 3 ),5.91(br,1H,OCH 2 O),5.95(br,2H,OCH 2 O),6.02(br,2...
experiment example (2
[0048] Experimental example (2) Preparation process and structural identification data of compound 2
[0049] Dissolve isotropine hydrochloride (1.0g, 2.81mmol) in 80ml of chloroform in a reaction flask, add NaH (450mg, 18.75mmol) under ice, slowly warm up to room temperature and stir the reaction for 24h, then concentrate the reaction solution under reduced pressure to Obtain a residue; first add ethyl acetate to the residue, then add an appropriate amount of pure water, extract 3 times with ethyl acetate, combine the ethyl acetate extracts, and use anhydrous MgSO 4 Dry, filter, and evaporate the filtrate to dryness. The resulting crude product is purified by silica gel column chromatography, eluting with petroleum ether / ethyl acetate (3 / 1, v / v), and the eluted part is concentrated to obtain 8-trichloromethyldihydro 995 mg of isotropine yellow solid, yield 80.7%. 1 HNMR (500MHz, CDCl 3 )δ: 2.68 (d, J=15.5Hz, 1H, NCH 2 C H 2 ),3.35-3.40(m,1H,NCH 2 C H 2 ), 3.70 (t, J=8...
experiment example (3
[0050] Experimental example (3) Preparation process and structure identification data of compound 3
[0051] Dissolve berberine hydrochloride (2.0g, 5.38mmol) in 60ml chloroform in a reaction flask, add 24ml of concentrated ammonia water, stir and react at room temperature for 24h, then separate the chloroform layer, wash the chloroform solution with water twice, and wash with Anhydrous MgSO 4 After drying the chloroform solution, filter it, and evaporate the filtrate to dryness to obtain a residue; the residue is separated and purified by silica gel column chromatography, eluted with dichloromethane, and the eluent is evaporated to dryness to obtain 8-trichloromethyldihydroberberis The base is 1.775 g of light yellow solid, the yield is 78.9%. 1 H NMR (500MHz, CDCl 3 )δ: 2.73 (d, J=15.5Hz, 1H, NCH 2 C H 2 ),3.33(m,1H,NCH 2 C H 2 ),3.71(m,1H,NC H 2 CH 2 ),3.87(ov,4H,ArOCH 3 ,NC H 2 CH 2 ),3.94(s,3H,ArOCH 3 ),5.65(s,1H,CH-CCl 3 ),5.94(s,2H,OCH 2 O),6.08(br s,1...
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