反应详情

A suspension of 6.42 g ethyl 3,5-dimethyl-4-hydroxybenzoate, 5.5 g potassium iodide, 3.7 g 1-chloro-4-pentyne and 2.3 g powdered potassium hydroxide in 650 ml acetonitrile was heated at reflux under nitrogen for 16 hrs. The mixture was filtered, concentrated in vacuo and subjected to flash filtration (silica gel, 4:1 hexane/ethyl acetate) to give 7.4 g ethyl 3,5-dimethyl-4-(3-ethynylpropoxy)benzoate as a yellow oil.

1. temperaturewas heated
2. temperatureat reflux under nitrogen for 16 hrs
3. filtrationThe mixture was filtered
4. concentrationconcentrated in vacuo
5. filtrationsubjected to flash filtration (silica gel, 4:1 hexane/ethyl acetate)