反应详情

温度

90 °C

A mixture of 3-(2-Fluoro-4-iodo-phenylamino)-1H-pyrrolo[3,2-c]pyridine-2-carboxylic acid ethyl ester (234 mg, 0.55 mmol), potassium carbonate (91 mg, 0.66 mg), sodium iodide (103 mg, 0.69 mmol) and 1-bromo-2-methoxy-ethane (0.057 mL, 0.61 mmol) in DMF (5 mL) was stirred a 90° C. for 2 days. It was cooled to room temperature, diluted with water and extracted into ethyl acetate. The organic layer was separated then washed with water followed by brine, then dried (Na2SO4), filtered and concentrated to give a residue which was purified by flash chromatography (Si-PPC, ether:pentane, gradient 20:80 to 50:50) to provide the title compound as a yellow oil (44 mg, 16%). LCMS (method B): RT=2.56 min, M+H+=483.

1. temperatureIt was cooled to room temperature
2. extractionextracted into ethyl acetate
3. customThe organic layer was separated
4. washthen washed with water
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customto give a residue which
9. customwas purified by flash chromatography (Si-PPC, ether:pentane, gradient 20:80 to 50:50)