Methods of treatment using a jak inhibitor compound
A composition and drug technology, applied in the direction of medical preparations containing active ingredients, drug combination, drug delivery, etc., can solve the problems of undisclosed compound 1
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example 1
[0188] Example 1: 5-Ethyl-2-fluoro-4-(3-(5-(1-methylpiperidin-4-yl)-4,5,6,7-tetrahydro-1H-imidazo[4 ,5-c]pyridin-2-yl)-1H-indazol-6-yl)phenol crystalline hydrate
[0189]
[0190]To a 3 L flask was added NMP (239 mL) and 5-ethyl-2-fluoro-4-(3-(4,5,6,7-tetrahydro-1H-imidazo[4,5-c] Pyridin-2-yl)-lH-indazol-6-yl)phenol 2HCl (74.5 g, 165 mmol) followed by addition of NMP (74 mL). Acetic acid (31.3 mL) was added and the reaction mixture was warmed to 55 °C for 10 min and then cooled to 25 °C. 1-Methylpiperidin-4-one (61.0 mL, 496 mmol) was added in one portion and the reaction mixture was stirred at 25 °C for 30 min and cooled to 15 °C. Sodium triacetoxyborohydride (98 g, 463 mmol) was added and after 5 min the external jacket was set to 20°C. After 3 h, ammonium hydroxide (365 mL, 5790 mmol) was added dropwise over 45 min, maintaining the temperature below 25 °C. The reaction mixture was stirred at 20 °C for 1.5 h, resulting in the formation of an off-white slurry. Methano...
example 2
[0192] Example 2: Powder X-ray Diffraction
[0193] with a Bruker D8-Advance X-ray diffractometer, using Cu-Kα radiation The powder X-ray diffraction (PXRD) pattern of the product of Example 1 was obtained at an output voltage of 45 kV and a current of 40 mA. The instrument was operated in Bragg-Brentano geometry, where the incidence, divergence and scattering slits were set to maximize the intensity at the sample. For measurements, a small amount of powder (5-25 mg) was gently pressed onto the sample holder to form a smooth surface, and subjected to X-ray exposure. The sample was scanned in 2Θ from 2° to 40° in 2Θ-2Θ mode with a step size of 0.02° and a scanning speed of 0.30° sec per step. Data acquisition was controlled by Bruker DiffracSuite measurement software and analyzed by Jade software (version 7.5.1). The instrument was calibrated within ±0.02° 2Θ with corundum standards. The observed PXRD 2Θ peak positions and d-spacings are shown in Table 1.
[0194] Table 1...
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