反应详情

(rac)-1-(6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-1-quinolin-6-yl-ethanol (Stage 154.1, 50 mg, 0.154 mmol) was dissolved in acetic acid >99% (0.150 mL) and sulfuric acid conc. 98% (0.050 mL) and the mixture was heated to reflux for 1 h. After cooling down to rt, ice water was added. The mixture was basified with NaOH 1 N and extracted with EtOAc twice. Combined organic layers were washed with brine and dried on Na2SO4. After evaporation of the solvent the crude was purified by preparative HPLC with acetonitrile/water (with 0.1% TFA) to afford the title compound as a yellow solid (tR 1.10 min (conditions 1), (MH+=307).

1. temperatureto reflux for 1 h
2. extractionextracted with EtOAc twice
3. washCombined organic layers were washed with brine
4. customdried on Na2SO4
5. customAfter evaporation of the solvent the crude
6. customwas purified by preparative HPLC with acetonitrile/water (with 0.1% TFA)