HRID1733266

反应详情

EQUATION

反应方程式

HRID 1733266 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

35 g of 3-(p-tert.butyl-phenyl)-2-methyl-allyl bromide in 70 ml of ether are added dropwise to a solution of 24.5 g of piperidine in 100 ml of absolute ether and the mixture is heated at reflux for 16 hours. The piperidine hydrobromide is removed by filtration and rinsed with ether. The ether solution is extracted with 2-N hydrochloric acid and made alkaline with 50% sodium hydroxide. The alkaline-aqueous solution is again extracted with ether, washed with water, dried over sodium sulphate and evaporated. By distillation there is obtained pure 1-[3-(p-tert.butyl-phenyl)-2-methyl-2-propenyl]-piperidine of boiling point 96°-98° C./0.03 Torr.

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 16 hours
  3. customThe piperidine hydrobromide is removed by filtration
  4. washrinsed with ether
  5. extractionThe ether solution is extracted with 2-N hydrochloric acid
  6. extractionThe alkaline-aqueous solution is again extracted with ether
  7. washwashed with water
  8. dry with materialdried over sodium sulphate
  9. customevaporated
  10. distillationBy distillation there