反应详情

温度

80 °C

A mixture of 1-(2-diethylaminoethyl)-4-trifluoromethyl-6-iodo-3-hydroxy-3-(2-naphthyl)oxindole of Example 48 (582 mg, 1, 24 mmol), 60% Zn(CN)2 (172 mg, 0.879 mmol), and (PPh3)4Pd (177 mg, 0.153 mmol) in DMF (6 mL) was stirred for 2.5 h at 80° C. Sat. aqueous NaHCO3 was added. The mixture was extracted with toluene-ethyl acetate, and the extracts were washed with sat. aq. NaHCO3, dried over MgSO4, and concentrated. The residue was purified by silica gel column chromatography with 80:1 to 50:1 chloroform/methanol to give the title compound (382 mg, 66%).

1. extractionThe mixture was extracted with toluene-ethyl acetate
2. washthe extracts were washed with sat. aq. NaHCO3
3. dry with materialdried over MgSO4
4. concentrationconcentrated
5. customThe residue was purified by silica gel column chromatography with 80:1 to 50:1 chloroform/methanol