HRID634971

反应详情

EQUATION

反应方程式

HRID 634971 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

A solution of 0.055 mol of lithium diisopropylamide (LDA) in 100 ml tetrahydrofuran (THF) was cooled to −78° C. under an inert atmosphere, and 0.055 mol of methyl decanoate in THF was added dropwise with stirring. The mixture was allowed to warm over one hour to −20° C., then cooled again to −78° C. A solution of 1-bromo-2-butyne (0.050 mol) in THF (20 ml) was added dropwise, and the mixture allowed to warm to room temperature overnight. Aqueous 6N HCl (100 ml) was added, and the product extracted with ethyl ether, dried with anhydrous sodium sulfate, concentrated, and distilled in vacuo to provide methyl 2-(2-butynyl)decanoate as an oil.

WORKUP

后处理

  1. additionwas added dropwise
  2. temperatureto warm over one hour to −20° C.
  3. temperatureto warm to room temperature overnight
  4. extractionthe product extracted with ethyl ether
  5. dry with materialdried with anhydrous sodium sulfate
  6. concentrationconcentrated
  7. distillationdistilled in vacuo