HRID1973206

反应详情

EQUATION

反应方程式

HRID 1973206 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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, the palladium black was filtered off from the reaction mixture, and dioxane was distilled off from the filtrate. To the resulting residue were added 50 milliliters of water, 200 milliliters of acetone and 10 grams of silver oxide, and the mixture was heated under reflux for 72 hours. After filtrating off precipitate contained in the reaction mixture, acetone and water were distilled off from the filtrate. By distillation of the residual liquid a fraction boiling in the temperature range of 135°-145° C./4.0mmHg was collected, whereby 0.6 mole of hydroxycitronellol was obtained.

WORKUP

后处理

  1. customthe solution was subjected to hydrogenation reaction in a reactor
  2. customno more absorbed
  3. filtrationThen, the palladium black was filtered off from the reaction mixture, and dioxane
  4. distillationwas distilled off from the filtrate
  5. additionTo the resulting residue were added 50 milliliters of water, 200 milliliters of acetone and 10 grams of silver oxide
  6. temperaturethe mixture was heated
  7. temperatureunder reflux for 72 hours
  8. filtrationAfter filtrating off precipitate
  9. distillationwere distilled off from the filtrate
  10. distillationBy distillation of the residual liquid a fraction
  11. customboiling in the temperature range of 135°-145° C./4.0mmHg
  12. customwas collected