反应详情

温度

60 °C

To a stirred solution of N-(5-Bromo-2-iodo-benzyl)-N-(4-chloro-2-vinyl-phenyl)-acetamide (0.55 g, 1.5 mmol) and Et3N (0.63 mL, 4.5 mmol) in DMF (25 mL) was added PdCl2 (40 mg, 0.23 mmol) and the reaction was heated to 60° C. When the reaction was complete by HPLC the mixture was poured into H2O and extracted with Et2O. The Et2O layer was washed with H2O (2×20mL) and brine (20 mL), dried (MgSO4), filtered and concentrated in vacuo. The residue obtained was purified by flash chromatography eluting with CH2Cl2 to give 1-(8-Bromo-2-chloro-6H-dibenzo[b,f]azocin-5-yl)-ethanone (0.24 g, 60%).

1. extractionextracted with Et2O
2. washThe Et2O layer was washed with H2O (2×20mL) and brine (20 mL)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue obtained
7. customwas purified by flash chromatography
8. washeluting with CH2Cl2