Derivatives of 6-(6-nh-substituted-triazolopyridazine-sulfanyl) benzothiazoles and benzimidazoles, preparation thereof, use thereof as drugs, and use thereof as met inhibitors
An alkyl and group technology, applied in the field of 6-benzothiazole and 6-benzimidazole derivatives
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Embodiment 1
[0305] 3-[(2-amino-1,3-benzothiazol-6-yl)thio]-N-(tetrahydro-2H-pyran-4-yl)[1,2,4]triazolo[ 4,3-b]pyridazin-6-amine
[0306] a) 3-[(2-amino-1,3-benzothiazol-6-yl)thio]-N-(tetrahydro-2H-pyran-4-yl)[1,2,4]triazole And[4,3-b]pyridazin-6-amine can be prepared as follows:
[0307] The argon flow is 900mg thiocyanate 2-amino-1,3-benzothiazol-6-yl ester in 27cm 3 The mixture in ethanol was bubbled for 5 min. Add 21mg of potassium dihydrogen phosphate in succession at 2.7cm 3 Solution in water, 2.01 g DL-dithiothreitol and 1.21 g 3-chloro-N-(tetrahydro-2H-pyran-4-yl)[1,2,4]triazolo[4,3-b ] Pyridazin-6-amine. The reaction mixture was heated at 80 °C for 18 hours. The resulting suspension was cooled to 20°C and the precipitate was spin-filter-dried and washed with water. The resulting hydrochloride form of solid in 10cm 3 water and 5cm 3 Absorption in a mixture of 1N sodium hydroxide. The suspension was stirred at 20 °C for 10 minutes then the solid was dried by spin filtratio...
Embodiment 2
[0314] N-(6-{[6-(tetrahydro-2H-pyran-4-ylamino)[1,2,4]triazolo[4,3-b]pyridazin-3-yl]thio} -1,3-Benzothiazol-2-yl)acetamide
[0315] a) N-(6-{[6-(tetrahydro-2H-pyran-4-ylamino)[1,2,4]triazolo[4,3-b]pyridazin-3-yl]sulfur Base}-1,3-benzothiazol-2-yl)acetamide can be prepared as follows:
[0316] At 20°C the 0.212cm 3 Acetyl chloride was added to 300 mg 3-[(2-amino-1,3-benzothiazol-6-yl)thio]-N-(tetrahydro-2H-pyran-4-yl)[1,2,4 ]triazolo[4,3-b]pyridazin-6-amine (1a) and 0.42cm 3 Triethylamine in 6cm 3 solution in dichloromethane. After 20 hours, the reaction mixture was concentrated to dryness and the solid residue was purified by chromatography (with dichloromethane) on a Biotage Quad 12 / 25 (KP-SIL, 60A; 32-63 μM) by solid deposit (solid deposit). / (38 dichloromethane / 17 methanol / 2 ammonia water) 95 / 5 to 70 / 30 gradient for elution). This gave 176 mg of N-(6-{[6-(tetrahydro-2H-pyran-4-ylamino)[1,2,4]triazolo[4,3-b]pyridazin-3-yl ]thio}-1,3-benzothiazol-2-yl)acetamide in the...
Embodiment 3
[0320] N-(6-{[6-(tetrahydro-2H-pyran-4-ylamino)[1,2,4]triazolo[4,3-b]pyridazin-3-yl]thio} -1,3-Benzothiazol-2-yl)cyclopropanecarboxamide
[0321] a) N-(6-{[6-(tetrahydro-2H-pyran-4-ylamino)[1,2,4]triazolo[4,3-b]pyridazin-3-yl]sulfur Base}-1,3-benzothiazol-2-yl)cyclopropanecarboxamide can be carried out in a manner similar to Example 2a, but using 300 mg of 3-[(2-amino-1,3-benzothiazol-6-yl )thio]-N-(tetrahydro-2H-pyran-4-yl)[1,2,4]triazolo[4,3-b]pyridazin-6-amine (1a) at 3cm 3 The solution in pyridine and 0.138cm 3 Cyclopropanecarboxylic acid chloride, prepared after reaction at 20°C for 18 hours. This gave 292 mg of N-(6-{[6-(tetrahydro-2H-pyran-4-ylamino)[1,2,4]triazolo[4,3-b]pyridazin-3-yl ]thio}-1,3-benzothiazol-2-yl)cyclopropanecarboxamide in the form of a beige powder characterized as follows:
[0322] 1H NMR spectrum (400MHz, DMSO-d6) δ.ppm 0.89-1.00 (m, 4H) 1.18-1.33 (m, 2H) 1.58-1.70 (m, 2H) 1.93-2.03 (m, 1H) 3.19-3.28 (m , 2H) 3.46-3.61 (m, 1H) 3.69 (d, J = 11....
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