反应详情

To a solution of 6-iodo-1H-indazole-3-carboxylic acid (3.00 g, 10.42 mmol) in dry DMF (50 mL) at 0° C. under an atmosphere of nitrogen was introduced sodium hydride (1.25 g of a 60% dispersion in mineral oil, 31.25 mmol). The reaction mixture was warmed to RT for 15 mins. 4,6-Dichloropyrimidin-2-amine (2.56 g, 15.62 mmol) was then added, and the solution warmed to 60° C. for 18 hr. After cooling to 0° C., the reaction was carefully quenched with water (50 mL) and acidified by addition of 0.5M aqueous citric acid. The resulting precipitate was collected by filtration, washed on the filter with 1:1 methanol/EtOAc and dried under vacuum to furnish the title compound as a beige solid: LC-MS: m/z=+415.85/417.90 (M+H)+. This compound, with LC-MS purity=70% UV, was used in the next step without further purification.

1. temperaturethe solution warmed to 60° C. for 18 hr
2. temperatureAfter cooling to 0° C.
3. customthe reaction was carefully quenched with water (50 mL)
4. additionacidified by addition of 0.5M aqueous citric acid
5. filtrationThe resulting precipitate was collected by filtration
6. washwashed on the
7. filtrationfilter with 1:1 methanol/EtOAc
8. customdried under vacuum