反应详情

温度

100 °C

To a solution of iii (165 mg, 0.626 mmol) in 1,4-dioxane (12 mL) was added ii (193 mg, 0.417 mmol) and PdCl2(dppf) (34 mg, 0.042 mmol). A solution of Cs2CO3 (410 mg, 1.30 mmol) in H2O (3 mL) was added, the reaction vessel sealed, then evacuated/purged with argon (×3). The mixture was then heated under microwave irradiation at 100° C. for 30 min. LCMS analysis indicated complete conversion. The mixture was diluted with EtOAc (100 mL), washed with H2O, brine, then separated and dried (Na2SO4). The organic fraction was concentrated in vacuo. Purification by chromatography on silica, eluting with 0-10% MeOH/EtOAc followed by additional chromatography on silica, eluting with 0-10% MeOH/DCM afforded Compound 5 (9 mg, 5%).

1. customthe reaction vessel sealed
2. customevacuated/purged with argon (×3)
3. additionThe mixture was diluted with EtOAc (100 mL)
4. washwashed with H2O, brine
5. customseparated
6. dry with materialdried (Na2SO4)
7. concentrationThe organic fraction was concentrated in vacuo
8. customPurification by chromatography on silica
9. washeluting with 0-10% MeOH/EtOAc
10. washeluting with 0-10% MeOH/DCM afforded Compound 5 (9 mg, 5%)