反应详情

温度

25 °C

A solution of 4.2 g (19 mmol) of the compound of step A in tetrahydrofuran (20 mL) was treated with carbonyldiimidazole (3.2 g, 19 mmol). The mixture was stirred at 25° C. for 16 h. Some precipitated imidazole was filtered off and the filtrate was concentrated under reduced pressure. The residue was partitioned between 1N HCl (20 mL) and ethyl acetate (50 mL). The organic layer was dried over magnesium sulfate and concentrated to an oil which solidified to give 3.8 g of the title compound of Step B as a solid melting at 104-107° C. It was used directly for the next step without further purification.

1. filtrationSome precipitated imidazole was filtered off
2. concentrationthe filtrate was concentrated under reduced pressure
3. customThe residue was partitioned between 1N HCl (20 mL) and ethyl acetate (50 mL)
4. dry with materialThe organic layer was dried over magnesium sulfate
5. concentrationconcentrated to an oil which