HRID1607817

反应详情

EQUATION

反应方程式

HRID 1607817 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe mixture was refluxed until complete dissolution
  2. temperatureIt was then cooled
  3. extractionextracted with ether (3×50 ml)
  4. washThe organic extracts were washed with 20% aqueous sodium hydroxide solution and water
  5. dry with materialdried over sodium sulfate
  6. customevaporated in vacuo
  7. customThe residue was purified by column chromatography on 50 g of silica gel