反应详情

温度

120 °C

A mixture of 3-(1-(2,3-difluorophenyl)-1H-tetrazol-5-yl)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-amine (2.50 g, 6.3 mmol), ethyl 2-bromo-4,5,7,8-tetrahydrothieno[3,2-d]azepine-6-carboxylate (1.91 g, 06.3 mmol), and NaHCO3 (15.6 mL, saturated solution in H2O) in N,N-dimethylformamide (83 mL) was degassed with a nitrogen stream for 20 min. To this mixture was added [1,1′-bis(diphenylphosphino)ferrocene]palladium (II) dichloride (460 mg, 0.6 mmol) and the reaction was stirred in a microwave for 10 min at 120° C. The resulting crude mixture was diluted with ethyl acetate (300 mL) and filtered. The filtrate washed with H2O (2×150 mL) and brine (1×150 mL), concentrated under reduced pressure, and purified via silica gel chromatography to provide ethyl 2-(6-amino-5-(1-(2,3-difluorophenyl)-1H-tetrazol-5-yl)pyridin-3-yl)-4,5,7,8-tetrahydrothieno[3,2-d]azepine-6-carboxylate.

1. customwas degassed with a nitrogen stream for 20 min
2. filtrationfiltered
3. washThe filtrate washed with H2O (2×150 mL) and brine (1×150 mL)
4. concentrationconcentrated under reduced pressure
5. custompurified via silica gel chromatography