HRID867084

反应详情

EQUATION

反应方程式

HRID 867084 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Activated zinc dust (15.0 g) was added to a stirred solution of 3-chloro-5,5-dimethylcyclohex-2-enone (9.0 g) and potassium iodide (7.5 g) in methanol (50 ml). After stirring for a period of 18 hours the mixture was filtered and the filtrate concentrated by evaporation under reduced pressure. The residue was mixed with dilute (8% w/v) hydrochloric acid and extracted with diethyl ether (2 × 100 ml). The combined ethereal extracts were washed with water and dried over anhydrous magnesium sulphate. After removal of the ether by evaporation under reduced pressure the residual oil was purified by distillation. 5,5-Dimethylcyclohex-2-enone was obtained as a pale yellow oil, b.p. 75° C./17 mm Hg.

WORKUP

后处理

  1. filtrationwas filtered
  2. concentrationthe filtrate concentrated by evaporation under reduced pressure
  3. additionThe residue was mixed
  4. additionwith dilute (8% w/v) hydrochloric acid
  5. extractionextracted with diethyl ether (2 × 100 ml)
  6. washThe combined ethereal extracts were washed with water
  7. dry with materialdried over anhydrous magnesium sulphate
  8. customAfter removal of the ether
  9. customby evaporation under reduced pressure the residual oil
  10. distillationwas purified by distillation