反应详情

To a solution of (6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-[2-(2-trimethylsilanyl-ethoxymethyl)-2H-indazol-5-yl]-methanone (Stage 195.3, 539 mg, 1.259 mmol) in THF (50 mL) was added dropwise at rt a solution of methylmagnesium bromide in Et2O (3 M, 0.462 mL). After 30 min stirring, the RM was taken into EtOAc and washed with a 10% NaHCO3 solution and then with brine. The organic layer was dried over Na2SO4 and the solvent was evaporated. The residue was purified by flash chromatography (CombiFlash® Companion System®, with RediSep® silica gel column, n-hexane/EtOAc=95:5->0:100) to afford after recrystallisation in pentane with a little EtOAc the title compound as a light yellowish powder (tR 5.6 min (conditions 3), MH+=444).

1. washwashed with a 10% NaHCO3 solution
2. dry with materialThe organic layer was dried over Na2SO4
3. customthe solvent was evaporated
4. customThe residue was purified by flash chromatography (CombiFlash® Companion System®, with RediSep® silica gel column, n-hexane/EtOAc=95:5->0:100)
5. customto afford
6. customafter recrystallisation in pentane with a little EtOAc the title compound as a light yellowish powder (tR 5.6 min (conditions 3), MH+=444)