HRID280394

反应详情

EQUATION

反应方程式

HRID 280394 的结构方程式

PROCEDURE

实验过程

To a solution of trans-2-butene-1,4-diol (7.57 g, 85.9 mmole) and a catalytic quantity of p-toluenesulfonic acid in 700 ml of dry ether was added dihydropyran (6.73 ml, 71.6 mmole) at the rate of 1.5 ml/hour. After stirring for four days, the reaction mixture was washed with saturated sodium bicarbonate, and the organic layer was separated and dried over sodium sulfate and concentrated in vacuo to afford the crude product which was purified via flash chromatography (LPS-1 silica gel; ether-hexane 1:1) to provide the title compound (5.75 g).

WORKUP

后处理

  1. washthe reaction mixture was washed with saturated sodium bicarbonate
  2. customthe organic layer was separated
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customto afford the crude product which
  6. customwas purified via flash chromatography (LPS-1 silica gel; ether-hexane 1:1)