反应详情

温度

25 °C

To intermediate 16 (0.49 g, 1.09 mmol) in methanol (30 mL) were added potassium acetate (0.128 g, 1.3 mmol), thiophenol (0.5 mL) and wet 10% Pd/C (0.2 g). The reaction mixture was stirred at 25° C. under hydrogen atmosphere. After uptake of H2 (1 eq), the catalyst was filtered off and the filtrate was evaporated. The residue was dissolved in water and dichloromethane. The resulting mixture was successively extracted with dichloromethane dried over MgSO4 and concentrated. The residue was purified by column chromatography using dichloromethane/methanol. The title compound 24 was collected as a white powder (333 mg, 81%). m/z=377 (M+H)+.

1. filtrationAfter uptake of H2 (1 eq), the catalyst was filtered off
2. customthe filtrate was evaporated
3. dissolutionThe residue was dissolved in water
4. extractionThe resulting mixture was successively extracted with dichloromethane
5. dry with materialdried over MgSO4
6. concentrationconcentrated
7. customThe residue was purified by column chromatography
8. customThe title compound 24 was collected as a white powder (333 mg, 81%)