反应详情

With stirring, 1 gram of 5-phenylpentanol was added dropwise to a mixture of 0.25 g of sodium hydride (60% oil suspension) and 25 ml of dried benzene. The mixed solution is further stirred at ambient temperatures for one hour. A benzene solution of propiolic acid chloride is prepared by stirring a mixture of 0.62 g of sodium propiolate, 0.80 g of thionyl chloride, and 20 ml of dried benzene at ambient temperatures for five hours. The benzene solution of propiolic acid chloride thus prepared is added to the mixed solution, stirred at ambient temperatures for five hours, and refluxed for one hour. After the reaction is completed, the reaction solution is washed successively with water and a saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. After removal of the solvent under reduced pressure, the obtained residue is subjected to silicagel column chromatography to yield 5-phenylpentyl propiolate (compound 1).

1. stirringThe mixed solution is further stirred at ambient temperatures for one hour
2. stirringby stirring
3. additionis added to the mixed solution
4. stirringstirred at ambient temperatures for five hours
5. temperaturerefluxed for one hour
6. washthe reaction solution is washed successively with water
7. dry with materiala saturated sodium chloride solution, and dried over anhydrous magnesium sulfate
8. customAfter removal of the solvent under reduced pressure