9-alkyl-oxa-tetraza-cyclopentadiene [a] anthracene derivative used as anti-inflammatory agent and preparation method thereof
An anti-inflammatory drug and drug technology, applied in anti-inflammatory agents, drug combinations, antipyretics, etc., can solve problems such as regenerative anemia, nephrotoxicity reduction, and gastrointestinal damage
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preparation example 1
[0015] Preparation example 1: To prepare 9-(4-fluoro-phenyl)-5,8,9,10-tetrahydro-4H-7-oxa-2,3,9,11b-tetraaza-cyclopentadiene[a ] Anthracene (compound Id) as an example to introduce the general synthetic method for preparing compound (I).
[0016] Add 15mmol of p-fluoroaniline, 37% formaldehyde solution containing 60mmol of formaldehyde, and 30ml of ethanol into a 100ml round bottom flask, stir it at room temperature for 5min, add 10mmol of compound 3, and reflux for 24h. Evaporate the solvent under reduced pressure, add 30ml of dichloromethane, wash with 30ml of 1mol / L NaOH aqueous solution × 2, wash with 30ml of water, and wash with saturated 30ml of NaCl. The dichloromethane layer was collected and washed with anhydrous MgSO 4 dry. After the dichloromethane was evaporated to dryness under reduced pressure, the silica gel column was separated and purified (methanol:dichloromethane=1:80), and the crude product obtained was recrystallized with ethanol to obtain compound Id. ...
Embodiment A
[0017] Example A: Anti-inflammatory experiment of intraperitoneal injection in mouse ear swelling model
[0018] With 9-(4-fluoro-phenyl)-5,8,9,10-tetrahydro-4H-7-oxa-2,3,9,11b-tetraaza-cyclopentadiene[a] Anthracene (compound Id) is taken as an example to introduce the pharmacological experiment method of compound I. In the experiment, 30 Kunming mice were randomly divided into 3 groups with 10 mice in each group (compound group, positive control group, and blank group). Id at a dose of 100 mg / kg, ibuprofen at a dose of 100 mg / kg and DMSO of the same volume were injected intraperitoneally, respectively. After 0.5 hours, 20 μL of xylene was used to evenly smear the right auricle of the mouse, and the activity was measured 0.5 hours after the application (the anti-inflammatory activity of the drug was measured for 1 hour). The mice were sacrificed by neck dislocation, and then the circular ear pieces were removed at the corresponding places of the mouse's left and right auri...
Embodiment B
[0025] Example B: Oral anti-inflammatory experiment in mouse ear swelling model
[0026] In the experiment, 50 Kunming mice were randomly divided into 5 groups with 10 mice in each group. After oral administration for 0.5, 1.5, 2.5, 3.5 and 4.5 hours, 20 μL of xylene was used to evenly smear the right auricle of the mice. After 0.5 hours after the application Activity measurement, method is the same as embodiment A. The Id of compound group administration 100mg / kg dosage, the ibuprofen of positive control group administration 100mg / kg dosage, the CMC-Na aqueous solution of 1‰ of blank group administration same volume. The experimental results obtained from data processing showed that both Id and ibuprofen had the best anti-inflammatory activity at 3 hours, and the inhibition rates were 64.73% and 41.58% respectively.
[0027] On this basis, Id and ibuprofen were carried out to 50mg / kg anti-inflammatory activity assay in 3 hours, the experimental results showed that Id and i...
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