HRID567390

反应详情

EQUATION

反应方程式

HRID 567390 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
7.5 °C

PROCEDURE

实验过程

0.1 mols of magnesium turnings are suspended in 50 ml of THF and treated with some drops of a solution of 0.12 mols of vinyl bromide in 100 ml of THF with stirring and under nitrogen atmosphere. As soon as the Grignard starts to form, the mixture is is cooled to 5-10° C. and added with the remaining solution of vinyl bromide in 30 min. The mixture is then cooled to −60° C. and added with 0.09 mols of beta ionone in 100 ml of THF in 20 min. The mixture is left to warm to room temperature, then heated at 40° C. for 2 hours. After that, the reaction is quenched as above described and vinyl beta-ionol is recovered by double distillation under vacuum, to obtain 166 g of a product, corresponding to an about 84% yield, with purity higher than 90%, determined by NMR.

WORKUP

后处理

  1. customto form
  2. temperatureThe mixture is then cooled to −60° C.
  3. waitThe mixture is left
  4. temperatureto warm to room temperature
  5. temperatureheated at 40° C. for 2 hours
  6. customAfter that, the reaction is quenched as
  7. distillationvinyl beta-ionol is recovered by double distillation under vacuum