HRID596612

反应详情

EQUATION

反应方程式

HRID 596612 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-5 °C

PROCEDURE

实验过程

A suspension of 4.84 g. of sodium hydride (57% mineral oil dispersion) in 70 ml. of dry dimethyl sulfoxide is heated at about 65° C. under argon with stirring for 1 hour. Dry tetrahydrofuran (75 ml.) is added and the resulting solution is cooled to -5° C. Trimethylsulfonium iodide (19 g., 92.8 mmol) is added very slowly and stirring is continued for about 5 minutes. A solution of 12.6 g. (92.8 mmol) of p-methoxybenzaldehyde in 120 ml. of tetrahydrofuran is added and the temperature is maintained at -5° C. After addition is completed the mixture is allowed to warm to room temperature, poured into water and extracted with ether. The extract is washed with saturated sodium chloride solution, dried and evaporated to give p-methoxystyrene oxide.

WORKUP

后处理

  1. additionA suspension of 4.84 g
  2. stirringstirring
  3. waitis continued for about 5 minutes
  4. temperaturethe temperature is maintained at -5° C
  5. additionAfter addition
  6. temperatureto warm to room temperature
  7. extractionextracted with ether
  8. washThe extract is washed with saturated sodium chloride solution
  9. customdried
  10. customevaporated