HRID462382

反应详情

EQUATION

反应方程式

HRID 462382 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 21 g of 3-butyn-1-ol and 27 g of imidazole in 100 ml of dimethyl formamide was treated with 45 g of t-butyldimethylsilyl chloride in several portions over a one hour period. After stirring under nitrogen for 18 hours the reaction mixture was diluted with 500 ml of ice water. The resulting aqueous solution was extracted with 300 ml of ether and the ethereal solution washed with water and then brine. The ethereal solution was dried over potassium carbonate. Evaporation of the ether and distillation of the residue gave 47.6 g of 3-butyn-1-ol t-butyldimethylsilyl ether, bp 80°-83° C./25 mm.

WORKUP

后处理

  1. extractionThe resulting aqueous solution was extracted with 300 ml of ether
  2. washthe ethereal solution washed with water
  3. dry with materialThe ethereal solution was dried over potassium carbonate
  4. customEvaporation of the ether and distillation of the residue