反应详情

温度

120 °C

In a microwave reaction vessel was dissolved (R)-3-(6-chloro-3-nitro-pyridin-2-ylamino)-3-phenyl-propionic acid ethyl ester (0.75 g, 2.14 mmol) in DMF (12 ml). Added the zinc cyanide (0.15 g, 1.29 mmol) and tetrakis(triphenylphosphine)palladium(0) (0.25 g, 0.21 mmol). Reaction mixture was degassed using a stream of nitrogen and capped. Reaction was heated in a microwave at 120° C. for 1 hour and then stirred at room temperature for 72 hours. After this time the reaction was poured into water and EtOAc. The layers were separated and the aqueous phase was extracted with EtOAc (3×). The combined organics were dried (MgSO4), filtered and concentrated to give the crude product which was purified via silica gel flash column chromatography (12 g silica gel, 5-20% EtOAc/hexanes) to afford 0.70 g (96%) of the title compound.

1. customIn a microwave reaction vessel
2. customReaction mixture
3. customwas degassed
4. customcapped
5. customReaction
6. customThe layers were separated
7. extractionthe aqueous phase was extracted with EtOAc (3×)
8. dry with materialThe combined organics were dried (MgSO4)
9. filtrationfiltered
10. concentrationconcentrated
11. customto give the crude product which
12. customwas purified via silica gel flash column chromatography (12 g silica gel, 5-20% EtOAc/hexanes)