HRID634549
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
N-phenyldibenzo[b,d]furan-2-amine (5.0 g, 19.3 mmol), and 1-bromo-3-iodobenzene (10.9 g, 38.6 mmol) were mixed in 100 mL of toluene. The solution was bubbled with nitrogen for 15 min. Pd(OAc)2 (0.22 g, 1.0 mmol), triphenylphosphine (0.51 g, 1.9 mmol) and sodium t-butoxide (2.2 g, 23.1 mmol) were then added. The mixture was refluxed overnight under nitrogen. After cooling, the reaction mixture was filtered through celite/silica pad and the filtrate was concentrated under vacuum. The residue was then purified by column chromatography using DCM:hexane (1:1, v/v) as the eluent. 5.6 g (71%) of a yellow solid was obtained as the product.
WORKUP
后处理
- customThe solution was bubbled with nitrogen for 15 min
- temperatureThe mixture was refluxed overnight under nitrogen
- temperatureAfter cooling
- filtrationthe reaction mixture was filtered through celite/silica pad
- concentrationthe filtrate was concentrated under vacuum
- customThe residue was then purified by column chromatography