HRID873512

反应详情

EQUATION

反应方程式

HRID 873512 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(3-Formyl-4-methoxyphenyl)boronic acid (5.30 g, 29.5 mmol) and 5,5-dimethylcyclohexane-1,3-dione (8.26 g, 58.9 mmol) were added to a suspension of dodecylbenzenesulfonic acid (0.96 g, 2.94 mmol) in water (196 ml) at room temperature, and the mixture thus obtained was then stirred under heating to reflux for 5 hours. After air-cooling, a solid was collected from the reaction solution by filtration. The solid thus obtained was suspended in ethanol, and the solution thus obtained was then stirred under heating to reflux. After air-cooling, the solvent was distilled away from the reaction solution under reduced pressure. Diethyl ether was added to the residue thus obtained, and the solid thus generated was collected by filtration and was then dried to obtain the title compound (7.99 g, yield: 64%).

WORKUP

后处理

  1. customthe mixture thus obtained
  2. temperatureunder heating
  3. temperatureto reflux for 5 hours
  4. temperatureAfter air-cooling
  5. filtrationa solid was collected from the reaction solution by filtration
  6. customThe solid thus obtained
  7. customthe solution thus obtained
  8. stirringwas then stirred
  9. temperatureunder heating to reflux
  10. temperatureAfter air-cooling
  11. distillationthe solvent was distilled away from the reaction solution under reduced pressure
  12. additionDiethyl ether was added to the residue
  13. customthus obtained
  14. filtrationthe solid thus generated was collected by filtration
  15. customwas then dried