HRID461925

反应详情

EQUATION

反应方程式

HRID 461925 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In this preparation 1.0 mole of p-toluenesulfonyl chloride is dissolved in 700 ml. of pyridine at 0° C, under nitrogen, and then 0.5 mole of hex-5-yn-1-ol is added dropwise. The mixture is stirred for 2 hours and then 10 ml. of water is added slowly, keeping the temperature below 10° C. The pyridine is then removed by evaporation under vacuum and the residue poured into 1 liter of ethyl acetate, then washed twice with excess 2N aqueous hydrochloric acid, and then with water. The organic layer is separated and dried over anhydrous magnesium sulfate, filtered, and the filtrate then evaporated to dryness, under vacuum, affording hex-5-yn-1-ol tosylate.

WORKUP

后处理

  1. dissolutionis dissolved in 700 ml
  2. customthe temperature below 10° C
  3. customThe pyridine is then removed by evaporation under vacuum
  4. additionthe residue poured into 1 liter of ethyl acetate
  5. washwashed twice with excess 2N aqueous hydrochloric acid
  6. customThe organic layer is separated
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. customthe filtrate then evaporated to dryness, under vacuum