反应详情

To a suspension of NaH (10 mg, 0.25 mmol) in DMF (1.25 mL) at 0° C. under argon was added 5-[2-fluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-{[6-(hydroxymethyl)pyridin-2-yl]amino}thiophene-3-carboxamide (Example 48) (50 mg, 0.125 mmol) and the mixture was allowed to stir for 20 minutes. Iodoethane (29 mg, 0.19 mmol) was then added and the reaction was allowed to warm to room temperature and subsequently heated to 60° C. overnight. The reaction was cooled to ambient temperature, quenched by the addition of water, extracted with ethyl acetate and concentrated in vacuo. The crude residue was reverse phase HPLC (acteonitrile/water with formic acid as a modifier) to afford the title compound.

1. temperaturesubsequently heated to 60° C. overnight
2. temperatureThe reaction was cooled to ambient temperature
3. customquenched by the addition of water
4. extractionextracted with ethyl acetate
5. concentrationconcentrated in vacuo