反应详情

温度

130 °C

A solution of EXAMPLE 22C (932 mg, 2.591 mmol) in DMSO (13 mL) was treated with 4-fluorobenzonitrile (408 mg, 3.368 mmol) and K2CO3 (1.788 g, 12.955 mmol), heated at 130° C. for 4 hours, and filtered. The filtrate was partitioned between aqueous NaHCO3 and ethyl acetate. The aqueous layer was extracted with ethyl acetate. The combined extracts were dried (MgSO4), filtered, and concentrated. The residue was purified by silica gel column chromatography with 20% ethyl acetate/hexanes to provide the desired product. MS (ESI) m/e 388, 390 (M+H)+.

1. filtrationfiltered
2. customThe filtrate was partitioned between aqueous NaHCO3 and ethyl acetate
3. extractionThe aqueous layer was extracted with ethyl acetate
4. dry with materialThe combined extracts were dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by silica gel column chromatography with 20% ethyl acetate/hexanes