反应详情

温度

-40 °C

2,2,2-Trifluoro-N-(6-iodo-imidazo[1,2-a]pyridin-2-yl)-acetamide (Stage 153.2, 1 g, 2.82 mmol) was dissolved in THF (15 mL) and cooled down to −40° C. under nitrogen atm. iPrMgCl in THF (2 M, 2.8 mL) was added dropwise. After 1 h stirring, cold DMF (0.65 mL, 8.46 mmol) in THF (1 mL) was added and the RM warmed up to −10° C. in 4 h. NH4Cl solution was added and the mixture was 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 preparative HPLC with acetonitrile/water (with 0.1% TFA) to afford the title compound (tR 0.88 min (conditions 2), (MH+=258).

1. temperaturethe RM warmed up to −10° C. in 4 h
2. extractionthe mixture was extracted 3 times with EtOAc
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)