Triazolium salts as PAR1 inhibitors, production thereof, and use as medicaments
A R21, C-R1 technology, applied in the direction of drug combination, antipyretics, anti-inflammatory agents, etc.
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Embodiment 1
[1001]1-{2-[3-Acetylamino-5-(pentafluorothio)phenyl]-2-oxoethyl}-3-amino-6-ethoxy-[1,2,4]tri Azolo[4,3-b]pyridazine-1- Trifluoroacetate
[1002]
[1003] a) 3-nitro-5-pentafluorothiobenzoic acid
[1004]
[1005] 3-Pentafluorothiobenzoic acid (5.0 g) was dissolved in fuming nitric acid (20 ml) and stirred at room temperature with the removal of moisture. Concentrated sulfuric acid (3ml) was then added, and the mixture was stirred at 75°C. After stirring at 75°C for 5 hours, sulfuric acid (1.5 ml) was added, and after stirring at 75°C for 2 hours, the mixture was allowed to stand overnight. The mixture was then added to ice-water and stirred for 2 hours. The precipitate formed was filtered off with suction and dried under high vacuum. 4.2 g of 3-pentafluorothio-5-nitrobenzoic acid are obtained. The mother liquor is extracted 3 times with dichloromethane, the combined dichloromethane phases are dried over magnesium sulfate and the solvent is concentrated, thus obtai...
Embodiment 4
[1034] 3-Amino-1-[2-(3-tert-butyl-4-methoxy-5-(morpholin-4-yl)phenyl)-2-oxoethyl]-6-trifluoromethyl -[1,2,4]triazolo[4,3-a]pyridine-1- Trifluoroacetate
[1035]
[1036] Dissolve 6-trifluoromethyl-[1,2,4]triazolo[4,3-a]pyridin-3-ylamine hydrobromide (W1.301; 309mg) in a small amount of water, The potassium solution was basified and extracted 3 times with EA. The combined EA phases were dried over magnesium sulfate, filtered and concentrated. This gave 212 mg of the free base, which was dissolved in DMF (5 ml) at room temperature with stirring. 2-Bromo-1-(3-tert-butyl-4-methoxy-5-(morpholin-4-yl)phenyl)ethanone (01.003; 427 mg in 1 ml DMF was slowly added over 15 minutes solution). The mixture was stirred at room temperature for 7 hours, then allowed to stand overnight. It was then stirred at 40°C for 2 hours and at 60°C for 3 hours. The solvent was then removed and the residue was purified by preparative HPLC. Fractions containing the desired product were combined,...
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