HRID2051413

反应详情

EQUATION

反应方程式

HRID 2051413 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20.0 Grams of 8-hydroxy-5-methyl-1,2,3,4,4a,9a-hexahydro-9-fluorenone, 10.4 g of potassium hydroxide and 200 ml of methanol were refluxed under heating until a homogeneous solution was produced. The solution was left to stand and thereto was added 16.0 ml of allyl bromide. The mixture was again refluxed under heating for 3 hours. The reaction mixture was poured into ice water and the separated crystal was collected by filtration and washed with water and then with n-hexane. The thus obtained crystal was once dissolved in chloroform and dried with magnesium sulfate and thereafter the solvent was distilled off. The crystal was recrystallized from ethanol to obtain 14.6 g of 8-allyloxy-5-methyl-1,2,3,4,4a,9a-hexahydro-9-fluorenone.

WORKUP

后处理

  1. temperatureunder heating until a homogeneous solution
  2. customwas produced
  3. waitThe solution was left
  4. temperatureThe mixture was again refluxed
  5. temperatureunder heating for 3 hours
  6. filtrationthe separated crystal was collected by filtration
  7. washwashed with water
  8. dissolutionThe thus obtained crystal was once dissolved in chloroform
  9. dry with materialdried with magnesium sulfate
  10. distillationthe solvent was distilled off
  11. customThe crystal was recrystallized from ethanol