反应详情

Intermediate 6 (compound 24, 4.0 g, 5.3 mmol) was added to a microwave reaction tube containing zinc cyanide (0.93 g, 7.9 mmol) and tetrakis(triphenylphosphine) palladium(0) (1.2 g, 1.1 mmol) in N,N-dimethylformamide (30 mL). The capped reaction tube was placed in a microwave reactor (Biotage® Initiator™) and the mixture was irradiated at 160° C. for 15 min. After dilution with ethyl acetate, the organic layer was subsequently washed with water, 10 wt % potassium carbonate and brine prior to drying over magnesium sulfate. After filtration and concentration under reduced pressure, the residue was purified on a Biotage® purification apparatus (silica gel, 10 to 60% ethyl acetate in hexanes gradient) to yield the title compound (2.0 g, 2.7 mmol, 52%) as a white solid.

1. customThe capped reaction tube
2. customwas placed in a microwave reactor
3. custom(Biotage® Initiator™) and the mixture was irradiated at 160° C. for 15 min
4. washAfter dilution with ethyl acetate, the organic layer was subsequently washed with water, 10 wt % potassium carbonate and brine
5. dry with materialto drying over magnesium sulfate
6. filtrationAfter filtration and concentration under reduced pressure
7. customthe residue was purified on a Biotage® purification apparatus (silica gel, 10 to 60% ethyl acetate in hexanes gradient)