反应详情

A mixture of 4-bromobenzaldehyde (4.05 g), 1-but-3-ynyl-4-phenylpiperazine (Step A) (4.69 g), triethylamine (9.2 mL), bis (triphenylphosphine)palladium dichloride (0.31 g) and copper (I) iodide (0.08 g) in acetonitrile (100 mL) is degassed with nitrogen and stirred at room temperature for 16 hours. The solvent is evaporated and the residue is dissolved in dichloromethane (200 mL), washed with 2N sodium carbonate (150 mL), dried over MgSO4, filtered and evaporated to leave a brown oil. This oil is purified by MPLC on silica gel eluting with 15% then 30% ethyl acetate (EtOAc)/hexanes to give 4.2 g of the title compound as a yellow waxy solid.

1. customis degassed with nitrogen
2. customThe solvent is evaporated
3. dissolutionthe residue is dissolved in dichloromethane (200 mL)
4. washwashed with 2N sodium carbonate (150 mL)
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customevaporated
8. customto leave a brown oil
9. customThis oil is purified by MPLC on silica gel eluting with 15%