反应详情

(rac)-(6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-[2-(2-trimethylsilanyl-ethoxymethyl)-2H-indazol-5-yl]-methanol (Stage 195.4, 580 mg, 1.349 mmol) was dissolved in acetone (40 mL) and heated 1 h to reflux together with 2-iodoxybenzoic acid (1.133 g, 4.05 mmol). The RM was cooled down to rt and the acetone was removed under reduced pressure. The residue was mixed with 2 M NaOH solution and extracted with EtOAc. The combined organic layers were 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=50:50->0: 100) to afford the title compound as a light brown foam (tR 7.11 min (conditions 3), MH+=428).

1. temperatureheated 1 h
2. customthe acetone was removed under reduced pressure
3. additionThe residue was mixed with 2 M NaOH solution
4. extractionextracted with EtOAc
5. dry with materialThe combined organic layers were dried over Na2SO4
6. customthe solvent was evaporated
7. customThe residue was purified by flash chromatography (CombiFlash® Companion System®, with RediSep® silica gel column, n-hexane/EtOAc=50:50->0: 100)