HRID1588423

反应详情

EQUATION

反应方程式

HRID 1588423 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

9.61 g (50 mmol) 3-(4-Methoxycarbonylphenyl)propanal are dissolved, together with 8.3 ml (68 mmol) of trimethylchlorosilane and 18.1 ml (0.13 mol) of triethylamine, in 15 ml of absolute dimethyl formamide and the solution is heated under reflux for 2 hours under nitrogen. After cooling, the reaction mixture is diluted with a saturated bicarbonate solution and extracted with petroleum ether. The organic phase is washed 3 times with a saturated bicarbonate solution, dried with sodium sulphate and concentrated by evaporation. The residue is distilled under a high vacuum (distillation apparatus silylated). 11.06 g of a pale yellow, oily product are thus obtained in the form of a mixture of the cis- and trans-isomers.

WORKUP

后处理

  1. temperaturethe solution is heated
  2. temperatureunder reflux for 2 hours under nitrogen
  3. temperatureAfter cooling
  4. extractionextracted with petroleum ether
  5. washThe organic phase is washed 3 times with a saturated bicarbonate solution
  6. dry with materialdried with sodium sulphate
  7. concentrationconcentrated by evaporation
  8. distillationThe residue is distilled under a high vacuum (distillation apparatus silylated)
  9. custom11.06 g of a pale yellow, oily product are thus obtained in the form of a mixture of the cis- and trans-isomers