反应详情

Sodium hydride (60% suspension in mineral oil, 99 mg, 2.47 mmol) was added to a stirring solution of 3-(2-methylsulfanyl-pyrimidin-4-yl)-1H-indazole (520 mg, 2.15 mmol) in NMP at 0° C. The mixture was stirred for 15 min and then methyliodide (0.14 mL, 2.25 mmol) was added and the resulting mixture was stirred for 2 h. The reaction mixture was then poured into water and extracted twice with EtOAc. The combined organic extracts were dried over Na2SO4, filtered and evaporated under reduced pressure. The residue was purified by flash chromatography (hexane/EtOAc, 9/1) to give 415 mg of 1-methyl-3-(2-methylsulfanylpyrimidin-4-yl)-1H-indazole.

1. stirringthe resulting mixture was stirred for 2 h
2. extractionextracted twice with EtOAc
3. dry with materialThe combined organic extracts were dried over Na2SO4
4. filtrationfiltered
5. customevaporated under reduced pressure
6. customThe residue was purified by flash chromatography (hexane/EtOAc, 9/1)