HRID67030

反应详情

EQUATION

反应方程式

HRID 67030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To an ice-cooled solution of 63 g. of 1-octyn-3-ol in 300 ml. of dimethoxyethane is added under an inert atmosphere 312 ml. of 1.6 M n-butyllithium in hexane dropwise over 1 hour. To the mixture is then added 145 g. of methyl iodide and the resulting mixture is stirred at ambient temperatures for 24 hours and then heated to 60° C. for 1 hour. The mixture is cooled and poured into cold dilute hydrochloric acid. The organic phase is separated, washed with water and saturated brine, dried (Na2SO4), and evaporated to an oil, dried (Na2SO4), and evaporated to an oil. Fractional distillation of the oil in vacuo yields the product as a colorless oil.

WORKUP

后处理

  1. additionTo the mixture is then added 145 g
  2. temperatureThe mixture is cooled
  3. customThe organic phase is separated
  4. washwashed with water and saturated brine
  5. dry with materialdried (Na2SO4)
  6. customevaporated to an oil
  7. dry with materialdried (Na2SO4)
  8. customevaporated to an oil
  9. distillationFractional distillation of the oil in vacuo