反应详情

A solution of pent-4-ynoic acid (1.0 g, 10 mmol), iodobenzene (2.3 ml, 20 mmol), copper(I) iodide (75 mg, 0.40 mmol) and dichlorobis(triphenylphosphine)-platinum(II) (140 mg, 0.20 mmol) in 20 mL of diethylamine was stirred at rt for 3 days. The volatile material are evaporated by a rotary evaporator and the resulting residue was dissolved in 50 mL dichloromethane and washed with 1 M HCl (50 mL). The dichloromethane layer was dried over sodium sulfate and evaporated to dryness under vacuum. The residue was purified by column chromatography (ethyl acetate/dichloromethane) to afford 5-phenylpent-4-ynoic acid (0.49 g).

1. customThe volatile material are evaporated by a rotary evaporator
2. dissolutionthe resulting residue was dissolved in 50 mL dichloromethane
3. washwashed with 1 M HCl (50 mL)
4. dry with materialThe dichloromethane layer was dried over sodium sulfate
5. customevaporated to dryness under vacuum
6. customThe residue was purified by column chromatography (ethyl acetate/dichloromethane)