反应详情

温度

60 °C

To a solution of 3,5-dichloro-4-((1-cyclohexyl-2-oxopyrrolidin-3-yl)methyl)phenyl trifluoromethanesulfonate (Example 240) (1.34 g, 2.83 mmol) in THF (30 mL) in a round bottom flask was added 3-cyano-4-fluorophenylboronic acid (560 mg, 3.39 mmol), sodium carbonate (900 mg, 8.48 mmol) and water (10 mL). The mixture was stirred at 60° C. for 5 minutes, palladium tetrakis (163 mg, 0.14 mmol) was added. Reaction mixture was brought to 80° C. and stirred for 3 hours. Cooled and partitioned between ethyl acetate and HCL(1 N). Organic was separated, wash with water, brine; dry over sodium sulfate, filter, and concentrate. Purify by silica gel (25-50% ethyl acetate in hexane) to afford 1.10 g (88%) of the title compound: Mass spectrum (LCMS) m/z=445.0 (M+H).

1. customReaction mixture
2. customwas brought to 80° C.
3. stirringstirred for 3 hours
4. temperatureCooled
5. custompartitioned between ethyl acetate and HCL(1 N)
6. customOrganic was separated
7. washwash with water, brine
8. dry with materialdry over sodium sulfate
9. filtrationfilter
10. concentrationconcentrate
11. customPurify by silica gel (25-50% ethyl acetate in hexane)