反应详情

(rac)-(6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-[2-(2-trimethylsilanyl-ethoxymethyl)-2H-indazol-5-yl]-methanol (Stage 150.3, 134 mg, 0.296 mmol) was charged into a microwave vial together with DME (2 mL), 1-Methyl-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-1H -pyrazole (173 mg, 0.815 mmol), followed by 2 M Na2CO3 (0.300 mL) and PdCl2(PPh3)2 (20 mg). The RM was submitted to microwave irradiation at 150° C. for 30 min. After filtration and evaporation of the solvent, the residue was taken into EtOAc and washed with saturated aqueous sodium carbonate. The aqueous phase was again extracted 3 times with EtOAc. Combined organic layers were washed with brine and dried on Na2SO4. After evaporation of the solvent the crude was purified by flash chromatography (CombiFlash® Companion System®, with 12 g RediSep® silica gel column, DCM/MeOH=100:0->92:8) to afford the title compound (tR 1.17 min (conditions 2), MH+=476)

1. customirradiation at 150° C. for 30 min
2. filtrationAfter filtration and evaporation of the solvent
3. washwashed with saturated aqueous sodium carbonate
4. extractionThe aqueous phase was again extracted 3 times with EtOAc
5. washCombined organic layers were washed with brine
6. customdried on Na2SO4
7. customAfter evaporation of the solvent the crude
8. customwas purified by flash chromatography (CombiFlash® Companion System®, with 12 g RediSep® silica gel column, DCM/MeOH=100:0->92:8)