反应详情

温度

70 °C

A mixture of 2-(2-iodophenyl)propanamide I13 (12.4 g, 45.2 mmol), ethynyltriethylsilane (9.72 mL, 54.2 mmol), PdCl2(PPh3)2 (0.634 g, 0.904 mmol), tri-tert-butylphosphonium tetrafluoroborate (0.262 g, 0.904 mmol) and CuI (0.172 g, 0.904 mmol) in DMF (46 mL) was stirred under a nitrogen atmosphere at 70° C. for 4 hours. The volatiles were removed in vacuo and the crude residue was purified by silica gel column chromatography (Combiflash Rf, 0-30% EtOAc in cyclohexane) to give the title compound I14 as an orange oil (8.9 g, 68%). LCMS-B: rt 3.845 min; m/z 288 [M+H]+.

1. customThe volatiles were removed in vacuo
2. customthe crude residue was purified by silica gel column chromatography (Combiflash Rf, 0-30% EtOAc in cyclohexane)