Synthetic Route of 54962-75-3, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 54962-75-3 as follows.
3-(4-MetIzyI-1H-imidazo1-1-y1)5-(trifluorornethy1)ani1ine: A suspension of 3-bromo-5-(trifluorornethyl)aniline (4.8 g, 20 mmol), 4-methylimidazole (1.97 g, 24 mmol), potassium carbonate (3.04 g, 22 mmol), Cu (0.57 g, 3 mmol), and 8-hydroxyquinoline (0.44 g, 3 mrnol,) in dry DMSO (20 mL) in a pressure tube was degassed by bubbling N2 into the suspension for 10minutes while stirring. The tube was sealed tightly. The mixture was heated at 120 C (oil bath temperature) for 15 h. The mixture was cooled down to 45- 50C and 14% aq. NH4OH (20 mL) was added. The mixture was maintained at this temperature for I h. After cooling to rt, water and ethyl acetate were added. The aqueous layer was extracted with ethyl acetate and the combined organic layers were passed through a short silica gel column to remove most of green/blue Cusalts. The filtrate was dried over sodium sulfate and concentrated on a rotavap. The crude product was recrystallized from EtOAc/hexanes, giving pure pale yellow needles. The motherliquor was concentrated and the residue was purified on silica gel column (5% methanol/methylene chloride), yielding a second crop as pale yellow needles.
According to the analysis of related databases, 54962-75-3, the application of this compound in the production field has become more and more popular.
Reference:
Patent; ARIAD PHARMACEUTICALS, INC.; GOZGIT, Joseph, M.; RIVERA, Victor, M.; SHAKESPEARE, William, C.; ZHU, Xiaotian; DALGARNO, David, C.; WO2013/162727; (2013); A1;,
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