تفاعل #507
ord-2bf6474a05bf4e7793ad68ef44642c0b
معادلة التفاعل
المذيبات
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الإجراء التجريبي
A reaction mixture of 8-chloro-4-methyl-2-(2,2,2-trifluoroethyl)-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine (0.044 g, 0.09 mmol), 6-methoxy-5-(1-methyl-1H-pyrazol-4-yl)pyridin-2-amine (0.019 g, 0.09 mmol), Cs2CO3 (0.046 g, 0.14 mmol), Tri-t-butylphosphonium tetrafluoroborate (2.73 mg, 9.41 µmol) and Bis(dibenzylideneacetone)palladium (2.70 mg, 4.70 µmol) in DME (2 mL) was flushed with argon and stirred at rt overnight. No product according to LCMS. The reaction mixture was then run in the microwave at 120°C for 30 minutes. Have unreacted startingmaterial left. Ran the sample again at 120°C for 30 minutes. Doesn´t seem as if the microwave warmed the vial. Added Tri-t-butylphosphonium tetrafluoroborate (2.73 mg, 9.41 µmol) and Bis(dibenzylideneacetone)palladium (2.70 mg, 4.70 µmol) and ran the vial at 120°C for 1 hr. Reaction complete. The mixture was filtered through celite and washed with DCM. The solvent was evaporated and the crude prouduct was purified by silica flash chromatography using a gradient of metanol (0 to 5%) in dichloromethane giving N-(6-methoxy-5-(1-methyl-1H-pyrazol-4-yl)pyridin-2-yl)-4-methyl-2-(2,2,2-trifluoroethyl)-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepin-8-amine (0.036 g, 85 %).