反应详情

温度

100 °C

A mixture of tetrakis(triphenylphosphine)palladium (34.8 mg, 0.03 mmol), methyl 2,6-dichloro-4-iodonicotinate (100 mg, 0.301 mmol) and dicyanozinc (38.9 mg, 0.331 mmol) in DMF (2 mL) was stirred at 100° C. overnight under N2 atmosphere. To the resulting mixture were added H2O and EtOAc. The aqueous phase was extracted with EtOAc, and the combined organic layers were washed with H2O and brine, dried over MgSO4 and evaporated. The residue was purified by chromatography on SiO2 to give the title compound as a white solid (28 mg, 40%). 1H NMR (500 MHz, DMSO-d6) δ ppm 3.99 (s, 3 H), 8.44 (s, 1H).

1. extractionThe aqueous phase was extracted with EtOAc
2. washthe combined organic layers were washed with H2O and brine
3. dry with materialdried over MgSO4
4. customevaporated
5. customThe residue was purified by chromatography on SiO2