Crystalline forms of [1,2,4]triazolo[1,5-a]pyridine derivatives with antitumor activity
A technology of anti-tumor drugs and crystal forms, which is applied in the field of crystal forms of [1,2,4]triazolo[1,5-a]pyridine derivatives, which can solve the problems of low bioavailability, large toxic and side effects, exclusive Issues such as weak sex
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Embodiment 1
[0033] Example 1 2-amino-5-[4-(4-morpholinomethyl)phenyl]-[1,2,4]triazolo[1,5-a]pyridine (compound 1) crystal form A preparation of
[0034]
[0035] Add 2ml of water and 10ml of 1,4-dioxane into a 25ml round bottom flask, stir and mix well, then add 2.85g (9.40mmol) of 4-(4-morpholinomethyl) phenylboronic acid pinacid, K 2 CO 3 1.30g (0.63mmol), PdCl 2 dppf 0.34g (0.46mmol), 5-bromo-[1,2,4]triazol[1,5-a]pyridin-2-amine 2g (9.29mmol), stirred at room temperature for 10 minutes, the reaction solution was yellow; The reaction bottle was transferred to an oil bath for reflux at 90° C. After 1 hour, the reaction solution turned from yellow to black, and the reaction was continued for 3-5 hours until the reaction was detected by TLC (developing agent: 5% CH 3 OH / CH 2 Cl 2 ); then want to add 10ml water to the flask to terminate the reaction, transfer to a 50ml beaker, CH 2 Cl 2 Extract (3×50ml), combine the organic phases, add 1g of anhydrous magnesium sulfate, filter, ...
Embodiment 2
[0045] Example 2 2-iodo-5-[4-(4-morpholinomethyl)phenyl]-[1,2,4]triazolo[1,5-a]pyridine (compound 2) crystal form B preparation of
[0046]
[0047] Add 100mg (0.32 mmol) and 8 mL of acetonitrile, after the substrate was stirred and dissolved at room temperature, 500 mg (7.25 mmol) of sodium nitrite was added, stirred for 1 minute, and then slowly added dropwise the mixed solution prepared by 0.5 mL of 45% HI solution and 2 mL of acetonitrile solution. A reddish-brown gas was generated, and after stirring at room temperature for 2 hours, the same amount of HI acetonitrile solution was added to continue the reaction for 2-3 hours, and TCL monitoring indicated that the reaction ended (developing agent: 5% CH 3 OH / CH 2 Cl 2 ). Transfer the reaction solution to a 50mL beaker, and use K 2 CO 3 The solution (1g / 8mL) was adjusted to neutrality, and the color of the solution changed from black to yellow. CH 2 Cl 2 Extract the organic phase (3 × 20mL), combine the organic p...
Embodiment 3
[0056] Embodiment 3 Drug efficacy test of the compound of the present invention
[0057] Using the MTT assay, it is a yellow compound, a dye that accepts hydrogen ions, and can act on the respiratory chain in the mitochondria of living cells. Under the action of succinate dehydrogenase and cytochrome C, the tetrazolium ring is cracked to produce blue Formanzan crystals, the amount of formanzan crystals generated is only proportional to the number of viable cells, the formanzan crystals generated by reduction can be dissolved in dimethyl sulfoxide (DMSO), and the optical density (OD) value at 490nm is measured by a microplate reader. The number of living cells can be reflected.
[0058] 1. Experimental steps
[0059] Lung cancer cell lines: A549 and H1299.
[0060] Experimental supplies: lung cancer cell lines, tools required for cell culture, MTT and compound mother solution are 10mmol / L.
[0061] 1. Specific methods.
[0062] (3-1) A549 and H1299 cells were resuscitated, ...
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