反应详情

温度

120 °C

To a stirred solution of 1C (0.63 g, 1.85 mmol) and Et3N (0.78 mL, 5.55 mmol) in DMF (15 mL) was added PdCl2 (49 mg, 0.28 mmol) and the reaction was heated to 120° C. When the reaction was complete by HPLC, the mixture was poured into H2O and extracted with Et2O. The Et2O layer was washed with H2O (2×20 mL) and brine (20 mL), dried (MgSO4), filtered and concentrated in vacuo. The residue obtained was purified by flash chromatography (SiO2, 100% CH2Cl2 to 10% EtOAc/CH2Cl2) to give 1D (0.12 g, 21%). HPLC Rt=2.77 min. (Column: YMC ODS-A 4.6×50 mm (4 min.); Solvent A=10% MeOH, 90% H2O, 0.1% TFA; Solvent B=90% MeOH, 10% H2O, 0.1% TFA); LCMS Found: (M+H)+=303.

1. extractionextracted with Et2O
2. washThe Et2O layer was washed with H2O (2×20 mL) and brine (20 mL)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue obtained
7. customwas purified by flash chromatography (SiO2, 100% CH2Cl2 to 10% EtOAc/CH2Cl2)