反应详情

温度

95 °C

To the product of Step D Example 129 (30.0 mg, 0.0516 mmol, material in the TFA salt form) was added 1,4-dioxane (4 mL), ethanol (0.5 mL), KOH (0.272 mg, 4.92 mmol), H2O (0.6 mL) and H2O2 (0.21 g). The reaction was heated to 95° C. for 22 hours. The solution was concentrated and the residue was dissolved in ethyl acetate before washing with water, drying (Na2SO4) and concentrating. The residue was purified by preparative thin layer chromatography (20 cm×20 cm, 1000 μm, silica gel) eluting with 10.5% ethyl acetate/dichloromethane affording the product. MS (electrospray) m/e 485.2 MH+ (Rt=4.2 min LC/MS).

1. concentrationThe solution was concentrated
2. dissolutionthe residue was dissolved in ethyl acetate
3. washbefore washing with water
4. dry with materialdrying (Na2SO4)
5. concentrationconcentrating
6. customThe residue was purified by preparative thin layer chromatography (20 cm×20 cm, 1000 μm, silica gel)
7. washeluting with 10.5% ethyl acetate/dichloromethane affording the product