反应详情

A solution of 5.5 g (18.9 mmole) 2-iodo-5-methoxyphenyl-2-propanone (18.9 mmole), 4.15 ml (37.8 mmole) of phenylacetylene, 0.037 g cuprous iodide (1 mole percent) and 0.066 g of bis(triphenylphosphine)palladium (II) chloride (5 mole percent) in 60 ml of triethylamine was stirred for 18 hours under N2 at room temperature. The mixture was partitioned between water and ether. The ether layer was washed successively with cold hydrochloric acid solution, washed and brine. It was dried over MgSO4 and the solvent evaporated in vacuo to give 5.6 g (100% yield) of brown crystals. Recrystallization from methylcyclohexane afforded pure 1-[5-(methoxy)-2-(phenylethynyl)phenyl]-2-propanone, mp 60°-62° C.

1. customThe mixture was partitioned between water and ether
2. washThe ether layer was washed successively with cold hydrochloric acid solution
3. washwashed
4. dry with materialIt was dried over MgSO4
5. customthe solvent evaporated in vacuo