反应详情

温度

120 °C

A 10 mL reaction vessel was charged with compound 245 (83.0 mg, 306 μmol), compound 309 (135 mg, 306 μmol), tris(dibenzylideneacetone)dipalladium (0) (21.0 mg, 22.9 μmol), 4,5-bis(diphenylphosphino)-9,9-dimethyl-9H-xanthene (26.6 mg, 45.9 μmol), sodium t-butoxide (58.8 mg, 612 μmol), and dioxane (2.5 mL). The reaction was purged with argon and heated with microwave energy (300 W) for 2 hours at 120° C. The resulting solution was added to aqueous K2CO3 (30 mL) and extracted with dichloromethane+10% methanol (3×30 mL). The combined organics were dried (MgSO4) and evaporated to give a yellow oil. Silica gel chromatography (gradient elution hexanes/20-100% ethyl acetate) afforded compound 310 as a colorless oil (142 mg, 69%).

1. customA 10 mL reaction vessel
2. customThe reaction was purged with argon
3. additionThe resulting solution was added to aqueous K2CO3 (30 mL)
4. extractionextracted with dichloromethane+10% methanol (3×30 mL)
5. dry with materialThe combined organics were dried (MgSO4)
6. customevaporated
7. customto give a yellow oil
8. washSilica gel chromatography (gradient elution hexanes/20-100% ethyl acetate)