反应详情

温度

80 °C

Potash (8.1 g, 58.7 mmol) and Pd(PPh3)4 (1.7 g, 1.5 mmol) were added to a solution of compound 44 (7.51 g, 29.1 mmol) and 4-chloro-3-nitrobenzene (4.6 g, 29.1 mmol) in a mixture of dioxane (80 mL) and water (20 mL). The mixture obtained was heated under argon to 80° C., kept at this temperature for 16 h (TLC monitoring, eluent: hexane-ethyl acetate, 1:1), cooled, filtered through Celite, and evaporated. The resulting product was dissolved in CH2Cl2 and an insoluble residue was filtered off. The resulting product was evaporated with silica gel and purified on a short thick column (eluent: hexane-CH2Cl2100:0→0:100, CH2Cl2-ethyl acetate 100:0→50:50). Compound 45 (5.0 g) was isolated and used in the next step without purification.

1. customThe mixture obtained
2. filtrationfiltered through Celite
3. customevaporated
4. dissolutionThe resulting product was dissolved in CH2Cl2
5. filtrationan insoluble residue was filtered off
6. customThe resulting product was evaporated with silica gel
7. custompurified on a short thick column (eluent: hexane-CH2Cl2100:0→0:100, CH2Cl2-ethyl acetate 100:0→50:50)