反应详情

A solution of Example 120A (0.5 g, 2.2 mmol) in tetrahydrofuran (10 mL) was added Lawesson's reagent (0.53 g, 1.3 mmol). After stirring at room temperature for 5 hours, the reaction mixture was poured into ethyl acetate (50 mL). The organic layer was washed with saturated NaHCO3 aqueous solution and brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by column chromatography (Analogix® Intelliflash280™, SiO2, 0-100% of ethyl acetate in hexanes) to obtain 0.33 g of the title compound. MS (ESI+) M/Z 245 [M+H]+.

1. washThe organic layer was washed with saturated NaHCO3 aqueous solution and brine
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by column chromatography (Analogix® Intelliflash280™, SiO2, 0-100% of ethyl acetate in hexanes)