反应详情

温度

80 °C

To a solution of the compound from Example 3 (E1) (0.2 g, 0.64 mmol) and 3-iodonitrobenzene (Aldrich, 0.16 g, 0.64 mmol) in triethylamine (4 mL) under an argon atmosphere was added trace tetrakis(triphenylphosphine)palladium(0), copper(I) iodide and triphenylphosphine. The mixture was heated at 80° C. for 0.2 h, was cooled to room temperature and was concentrated in vacuo. The residue was partitioned between ethyl acetate and water. The organic phase was washed with brine, was dried (MgSO4) and was evaporated. Purification by flash chromatography, eluting with 3:1 hexanes/ethyl acetate, provided the title compound as yellow solid (0.25 g, 90%), m.p. 46°-48° C.

1. temperaturewas cooled to room temperature
2. concentrationwas concentrated in vacuo
3. customThe residue was partitioned between ethyl acetate and water
4. washThe organic phase was washed with brine
5. dry with materialwas dried (MgSO4)
6. customwas evaporated
7. customPurification by flash chromatography
8. washeluting with 3:1 hexanes/ethyl acetate