反应详情

Intermediate 10b (562 mg, 1.50 mmol), 2-methoxyacetamide (334 mg, 3.75 mmol), Xantphos (173 mg, 0.30 mmol) and potassium carbonate (518 mg, 3.75 mmol) were suspended in 1,4-dioxane (20 mL), warmed, degassed, and placed under argon. To this mixture palladium acetate (34.0 mg, 0.15 mmol) was added. The mixture was degassed and then heated at reflux for 17 h. After cooling, the mixture was filtered through Celite, washing with DCM, and evaporated to a yellow gum. Purification by FCC, eluting with 0-100% ethyl acetate in cyclohexane, gave the title compound as a white foam (281 mg, 44%). LCMS (Method 3): Rt 3.27 min, m/z 450.2 [MNa+].

1. temperaturewarmed
2. customdegassed
3. customThe mixture was degassed
4. temperatureheated
5. temperatureat reflux for 17 h
6. temperatureAfter cooling
7. filtrationthe mixture was filtered through Celite
8. washwashing with DCM
9. customevaporated to a yellow gum
10. customPurification by FCC
11. washeluting with 0-100% ethyl acetate in cyclohexane