HRID844619

反应详情

EQUATION

反应方程式

HRID 844619 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

56.1 g 3,7,11-trimethyl-1-dodecin-3-ol, 27.0 g isopropenyl methyl ether and 100 mL n-heptane were initially introduced into a 500 ml flask. 14.5 mg methanesulfonic acid were added, while stirring. The reaction mixture was stirred under reflux for 7.5 hours. During this period of time, 36.5 g isopropenyl methyl ether and 21.6 mg methanesulfonic acid were added in each case in two portions. The mixture was cooled to room temperature, neutralized with 3 ml methanolic NaOAc solution (10 g/1) and evaporated. The crude was hydrogenated with 10% Pd/C in isopropanol. Phytone was obtained in a yield of 91%.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred
  2. temperatureunder reflux for 7.5 hours
  3. customevaporated