HRID1607817
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
1.10 g of sodium hydroxide was added to a solution of 2.35 g of phenol in 20 ml of absolute ethanol. The mixture was refluxed until complete dissolution, then 2.92 g of 1-bromobut-2-yn-4-ol tetrahydropyranyl ether was added. The reflux was resumed for 2 additional hours. It was then cooled, poured into water and extracted with ether (3×50 ml). The organic extracts were washed with 20% aqueous sodium hydroxide solution and water, dried over sodium sulfate and evaporated in vacuo. The residue was purified by column chromatography on 50 g of silica gel, using hexane:ethyl acetate (98:2) as eluant, to yield 4-phenoxy-but-2-yn-1-ol tetrahydropyranyl ether, as an oil.
WORKUP
后处理
- temperatureThe mixture was refluxed until complete dissolution
- temperatureIt was then cooled
- extractionextracted with ether (3×50 ml)
- washThe organic extracts were washed with 20% aqueous sodium hydroxide solution and water
- dry with materialdried over sodium sulfate
- customevaporated in vacuo
- customThe residue was purified by column chromatography on 50 g of silica gel