HRID1290973

反应详情

EQUATION

反应方程式

HRID 1290973 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(2-Cyanopropyl)-4-(4-methoxybenzyl)cyclohexanone 1,4-Dioxospiro[4,5]decan-8-one (45.6 g) was added to a mixture of 4-methoxybenzyl triphenylphosphonium bromide (127.3 g) and epichlorohydrin (100 ml) in toluene (1500 ml) and heated at reflux under a nitrogen atmosphere for 36 hours. The solvent was evaporated under reduced pressure and the residue was extracted into hexane. The hexane solution was evaporated under reduced pressure and the residue distilled at 24° C./1 mmHg to give 8-(4-methoxybenzylidine)- 1,4-dioxaspiro[4,5]-decane, (19 g).

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux under a nitrogen atmosphere for 36 hours
  3. customThe solvent was evaporated under reduced pressure
  4. extractionthe residue was extracted into hexane
  5. customThe hexane solution was evaporated under reduced pressure
  6. distillationthe residue distilled at 24° C./1 mmHg