反应详情

In a reaction vessel were added tert-butyl [(2R)-2-hydroxy-2-phenylethyl][2-(4-iodophenoxy)ethyl]carbamate (200 mg), [3-isopropoxy-4-[[(methylsulfonyl)amino]carbonyl]-phenyl]boronic acid (150 mg), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II), complex with dichloromethane (1:1, 33.8 mg), toluene (3.2 ml), ethanol (0.8 ml), and 2N sodium carbonate solution (0.66 ml). The vessel was placed in a microwave and irradiation was adjusted to keep the temperature 100° C. and the reaction was performed for 2 hours. After cooling to room temperature, the mixture was quenched by the addition of 1N hydrochloric acid (1.32 ml) and partitioned between ethyl acetate (20 ml) and water (20 ml). The organic layer was separated, washed with brine (20 ml), and dried over magnesium sulfate. Filtration followed by evaporation gave a brown foam which was chromatographed on silica gel (eluent: hexane/ethyl acetate) to give tert-butyl [(2R)-2-hydroxy-2-phenylethyl]-[2-[[3′-isopropoxy-4′-[[(methylsulfonyl)amino]carbonyl]-4-biphenylyl]oxy]ethyl]carbamate (20.4 mg) as a pale yellow solid.

1. customThe vessel was placed in a microwave and irradiation
2. customthe temperature 100° C.
3. customthe mixture was quenched by the addition of 1N hydrochloric acid (1.32 ml)
4. custompartitioned between ethyl acetate (20 ml) and water (20 ml)
5. customThe organic layer was separated
6. washwashed with brine (20 ml)
7. dry with materialdried over magnesium sulfate
8. filtrationFiltration
9. customfollowed by evaporation
10. customgave a brown foam which
11. customwas chromatographed on silica gel (eluent: hexane/ethyl acetate)