تفاعل #518
ord-bf7cf9ac04cd4fedb1f93e4a263e0d2f
المذيبات
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الإجراء التجريبي
Palladium(II) acetate (0.019 g, 0.08 mmol) and 4,5-Bis(diphenylphosphino)-9,9-dimethylxanthene (0.096 g, 0.17 mmol) were added to a degassed solution of 8-chloro-2-(3,3-difluorocyclobutyl)-4-methyl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine (0.160 g, 0.55 mmol), 6-methoxy-5-(1-methyl-1H-pyrazol-4-yl)pyridin-2-amine (0.113 g, 0.55 mmol) and Cesium carbonate (0.058 mL, 0.72 mmol) in dry dioxane (15 mL). The reaction was heated in a microwave oven at 145°C for 1h. About 50% of product. The reaction was heated at 145°C for another 30 min. About 45% of product. The reaction was interrupted and the reaction mixture was pooled with the corresponding mixture in EN04426-52. The reaction mixture was filtered through a plug of celite. The celite was washed with DCM. The solvents were evaporated and the crude was purified by ISCO on a 25 g column with an increased gradient of DCM/MeOH (90/10) 0-50% in DCM) to give 0.176 g (35%) of the product. The enatiomers were also separated (see EN04426-56).