反应详情

To abs. MeOH (2 mL) stirred at rt were added 3-(6-fluoro-1-methyl-1H-indazol-5-ylmethyl)-6-(1-piperidin-4-yl-1H-pyrazol-4-yl)-imidazo[1,2-b]pyridazine (Example 282, 79 mg, 0.184 mmol), formaldehyde (0.068 mL, 0.918 mmol) and NaBH3CN (58 mg, 0.918 mmol). The RM was then brought to pH 5-6 with addition of acetic acid and stirred at rt for 2 h. It was then taken into EtOAc and washed with saturated NaHCO3 sol. The organic layer was then washed with brine, dried on Na2SO4, filtered and evaporated. The residue was then purified by preparative HPLC with acetonitrile and water (+0.1% TFA) to afford the title compound (tR 0.85 min (conditions 2), MH+=445).

1. washwashed with saturated NaHCO3 sol. The organic layer
2. washwas then washed with brine
3. customdried on Na2SO4
4. filtrationfiltered
5. customevaporated
6. customThe residue was then purified by preparative HPLC with acetonitrile and water (+0.1% TFA)