反应详情

To a solution of 6-bromo-N2-(2,3-dihydro-benzofuran-5-ylmethyl)-pyrazine-2,3-diamine (1.0 g, 3.12 mmol) in AcOH:H2O (8 mL: 8 mL) was added the solution of NaNO2 (2.12 g, 31.2 mmol) in water (5 mL). The mixture was stirred at room temperature for 1 hour, and then heated at 65° C. for 16 hours. The solvents were removed, and then EtOAc (20 mL) and water (20 mL) were added. The aqueous layer was extracted with EtOAc (3×20 mL). The combined extracts were dried over Na2SO4, concentrated and purified by silica gel chromatography with EtOAc: Hexanes to provide 6-bromo-1-(2,3-dihydro-benzofuran-5-ylmethyl)-1H-[1,2,3]triazolo[4,5-b]pyrazine (543 mg, 52% yield).

1. temperatureheated at 65° C. for 16 hours
2. customThe solvents were removed
3. additionEtOAc (20 mL) and water (20 mL) were added
4. extractionThe aqueous layer was extracted with EtOAc (3×20 mL)
5. dry with materialThe combined extracts were dried over Na2SO4
6. concentrationconcentrated
7. custompurified by silica gel chromatography with EtOAc