HRID1973205

反应详情

EQUATION

反应方程式

HRID 1973205 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1 mole of 7-chloro-3,7-dimethyl-3-octenyl acetate was dissolved into 200 milliliters of dioxane and the solution was subjected to hydrogenation reaction in a reactor containing 20 grams of activated palladium black at about 25° C. under normal pressure until hydrogen was no more absorbed. Then, palladium black was filtered off, from the reaction mixture and dioxane was distilled off from the filtrate under reduced pressure. The residual liquid was added to the solution of 40 grams of sodium hydroxide in 200 milliliters of methanol, and heated under reflux for 72 hours. The resulting reaction mixture was diluted with 1200 milliliters of water, and the oil layer was separated from the aqueous layer. The oil layer thus separated was washed with 200 milliliters of water three times and then dried over 20 grams of Glauber's salt (sodium sulfate). By distillation of the oil layer under reduced pressure a fraction having a boiling point range of 110°-118° C./15mmHg was collected, whereby 0.7 mole of citronellol was obtained.

WORKUP

后处理

  1. customthe solution was subjected to hydrogenation reaction in a reactor
  2. customno more absorbed
  3. filtrationThen, palladium black was filtered off, from the reaction mixture and dioxane
  4. distillationwas distilled off from the filtrate under reduced pressure
  5. additionThe residual liquid was added to the solution of 40 grams of sodium hydroxide in 200 milliliters of methanol
  6. temperatureheated
  7. temperatureunder reflux for 72 hours
  8. customThe resulting reaction mixture
  9. customthe oil layer was separated from the aqueous layer
  10. customThe oil layer thus separated
  11. washwas washed with 200 milliliters of water three times
  12. dry with materialdried over 20 grams of Glauber's salt (sodium sulfate)
  13. distillationBy distillation of the oil layer under reduced pressure a fraction
  14. customa boiling point range of 110°-118° C./15mmHg
  15. customwas collected