反应详情

温度

100 °C

To a solution of compound 10D (0.5 g, 1.94 mmol) in a mixed solvent of DMF (2.5 mL) and water (1.9 mL) was added Cu(OAc)2 (1.057 g, 5.82 mmol), followed by a 10 M aqueous solution of LiCl (0.58 mL, 5.8 mmol) and PdCl2 (34.3 mg, 0.194 mmol). The resulting suspension was heated to 100° C. for 1 h. After cooling to rt, the reaction mixture was poured into ice/water, and extracted with EtOAc (3×). The combined EtOAc extracts were washed with brine, dried (Na2SO4), and concentrated under reduced pressure. The crude product was chromatographed (silica gel) eluting with 10% to 50% EtOAc/hexane to furnish the title compound (0.3 g) as a white foam.

1. temperatureAfter cooling to rt
2. extractionextracted with EtOAc (3×)
3. washThe combined EtOAc extracts were washed with brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated under reduced pressure
6. customThe crude product was chromatographed (silica gel)
7. washeluting with 10% to 50% EtOAc/hexane