反应详情

The product of step A (150 mg, 0.398 mmol), acetamide (101 mg, 1.71 mmol) and Pd(OAc)2 (13.4 mg, 0.02 mmol) in THF (4.5 mL) and H2O (1.5 mL) was heated at 65° C. for 24 h. The mixture was cooled to RT and diluted with H2O. The solution was extracted with EtOAc (×3). The combined organic layers were washed with brine (1×), dried over anhydrous MgSO4, filtered, and concentrated under vacuum to leave a residue which was purified by silica gel column chromatography (elution with 20:1 DCM:MeOH) to yield the desired compound. MS (ESI) m/z 395 [M+H]+.

1. extractionThe solution was extracted with EtOAc (×3)
2. washThe combined organic layers were washed with brine (1×)
3. dry with materialdried over anhydrous MgSO4
4. filtrationfiltered
5. concentrationconcentrated under vacuum
6. customto leave a residue which
7. customwas purified by silica gel column chromatography (elution with 20:1 DCM:MeOH)