反应详情

温度

0 °C

To a solution of 4-iodo-7-azaindazole (Potashman et.al., WO2005070891) (123 mg) in THF (2 mL) at 0° C. was added isopropylmagnesium chloride (2 M solution in THF, 0.5 mL). The mixture was stirred at 0° C. for 30 min and 5-chloro-3-(4-chloro-3-trifluoromethyl-benzenesulfonylamino)-pyridine-2-carboxylic acid methoxy-methyl-amide (114 mg) was added. The reaction mixture was warmed to room temperature, stirred for 2 h and quench by saturated aqueous NH4Cl solution (2 mL). The organic layer was separated and the aqueous layer was extracted with EtOAc (5 mL). The combined organic layers were dried (Na2SO4), filtered and evaporated in vacuo. The residue was purified by flash chromatography (silica) to afford the title compound as a white powder. MS (M+H)+: 515.9.

1. temperatureThe reaction mixture was warmed to room temperature
2. stirringstirred for 2 h
3. customquench by saturated aqueous NH4Cl solution (2 mL)
4. customThe organic layer was separated
5. extractionthe aqueous layer was extracted with EtOAc (5 mL)
6. dry with materialThe combined organic layers were dried (Na2SO4)
7. filtrationfiltered
8. customevaporated in vacuo
9. customThe residue was purified by flash chromatography (silica)