反应详情

温度

110 °C

To a solution of tert-butyl (3-((3-bromopyridin-2-yl)oxy)cyclobutyl)carbamate (see PREPARATION 7B; 343 mg, 1 mmol), 4-(3,3,4,4-tetramethyl-borolan-1-yl)-3,6-dihydro-2H-pyran (2.27 mg, 1.1 mmol) and K3PO4 (424 mg, 2 mmol) in 1,4-dioxane (60 mL) and H2O (6 mL) was added Pd(dppf)Cl2 (36.6 mg, 0.05 mmol) then the reaction mixture was stirred at 110° C. under N2 for overnight. The reaction mixture was filtered through CELITE® and washed with CH2Cl2. The organic layer was concentrated and the crude product was purified by silica gel column to give tert-butyl (3-((3-(3,6-dihydro-2H-pyran-4-yl)pyridin-2-yl)oxy)cyclobutyl)carbamate (242 mg, 0.7 mmol, yield 70%). ESI-MS (M+1): 347 calc. for C19H26N2O4 346

1. filtrationThe reaction mixture was filtered through CELITE®
2. washwashed with CH2Cl2
3. concentrationThe organic layer was concentrated
4. customthe crude product was purified by silica gel column