反应详情

温度

120 °C

To a solution of 3-amino-5-(2,2-difluoro-ethylamino)-6-trimethylsilanylethynyl-pyrazine-2-carboxylic acid methyl ester (624 mg, 1.9 mmol) in DMF (19 ml) was added Copper(I) iodide (181 mg, 0.95 mmol) and the mixture was heated to 120° C. for 2 h. The reaction mixture was filtered through Hyflo, the residue washed with toluene. The combined organic phases were extracted with water, dried with Na2SO4 and evaporated. The residue was purified by chromatography on silica gel (cyclohexane to cyclohexane/EtOAc 40:60) to provide the title compound as yellow solid.

1. filtrationThe reaction mixture was filtered through Hyflo
2. washthe residue washed with toluene
3. extractionThe combined organic phases were extracted with water
4. dry with materialdried with Na2SO4
5. customevaporated
6. customThe residue was purified by chromatography on silica gel (cyclohexane to cyclohexane/EtOAc 40:60)