HRID1563

反应详情

EQUATION

反应方程式

HRID 1563 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 5.0 g of 2-butyne-1,4-diol and 10 milligrams of p-toluenesulfonic acid and 150 ml of dry ether there was added dropwise with stirring at room temperature 4.9 g of 3,4-dihydro-2H-pyran. After stirring overnight at ambient temperature the ether was evaporated and the residue was poured into 200 ml of water. The aqueous solution was extracted with hexane (2×100 ml) and then re-extracted with ether (3×100 ml). The combined ether extracts were washed with 100 ml of brine, dried over magnesium sulfate and evaporated to yield 6.8 g of 4-tetrahydropyranoxy-2-butyn-1-ol.

WORKUP

后处理

  1. additionwas added dropwise
  2. customwas evaporated
  3. additionthe residue was poured into 200 ml of water
  4. extractionThe aqueous solution was extracted with hexane (2×100 ml)
  5. extractionre-extracted with ether (3×100 ml)
  6. washThe combined ether extracts were washed with 100 ml of brine
  7. dry with materialdried over magnesium sulfate
  8. customevaporated