反应详情

温度

140 °C

A mixture of 4-chloro-5-iodo-6-methylpyrimidin-2-ylamine (1.35 g, 5.0 mmol), zinc cyanide (288 mg, 2.45 mmol) and tetrakis(triphenylphosphine)palladium (290 mg, 5 mol %) in DMF (20 mL) was purged with argon gas and heated at 140° C., for 15 min, by microwave irradiation. After cooling to RT, the residue was partitioned between EtOAc and water. The aqueous phase was further extracted with EtOAc and the combined organic fractions washed with brine, dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, gradient 0-30% EtOAc in DCM) followed by further column chromatography (Si—PCC, gradient 0-7% MeOH in DCM) to afford the title compound (40 mg, 5%) as a pale yellow solid. LCMS (Method C): RT 2.23 min [M+H]+ 169.00. 1H NMR (DMSO-d6, 400 MHz): δ 8.11 (2H, br s), 2.42 (3H, s)

1. customwas purged with argon gas
2. temperatureAfter cooling to RT
3. customthe residue was partitioned between EtOAc and water
4. extractionThe aqueous phase was further extracted with EtOAc
5. washthe combined organic fractions washed with brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated in vacuo
8. customThe resulting residue was purified by column chromatography (Si—PCC, gradient 0-30% EtOAc in DCM)