反应详情

温度

100 °C

The product of example 54 (step A) (500 mg, 1.17 mmol), Pd2(dba)3 (43 mg, 0.046 mmol), dppf (51.5 mg, 0.093 mmol), Zn(CN)2 (89 mg, 0.755 mmol) and zinc dust (18 mg, 0.278 mmol) in DMA (1 mL) was evacuated and back-filled with argon (×3). The mixture was stirred at 100° C. for 4 h. The reaction was cooled to room temperature, diluted with Et2O and filtered through a pad of silica. The filtrate was concentrated under vacuum to leave a residue which was purified by silica gel column chromatography (elution with 5:1 hexane:ethyl acetate) to yield the title compound as a colorless gum. MS (ESI) m/z 377 [M+H]+.

1. additionback-filled with argon (×3)
2. temperatureThe reaction was cooled to room temperature
3. filtrationfiltered through a pad of silica
4. concentrationThe filtrate was concentrated under vacuum
5. customto leave a residue which
6. customwas purified by silica gel column chromatography (elution with 5:1 hexane:ethyl acetate)