HRID1077140

反应详情

EQUATION

反应方程式

HRID 1077140 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add a mixture of 1-diethylamino-6-(m-methoxyphenyl)-5-methylhexan-3-one and 5-methyl-6-(m-methoxyphenyl)hex-1-en-3-one (6 g, prepared by slow distillation of the former substance) to 2-ethylcyclopentane-1,3-dione (3.5 g) in 0.12% methanolic potassium hydroxide (10 cc) and heat the mixture under reflux for 6 hours. Remove most of the solvent under reduced pressure and add ether (25 cc) and benzene (25 cc) to the residue. Wash the solution with 5% aqueous sodium hydroxide, water, dilute hydrochloric acid, and brine, and dry. Evaporate the solvent to obtain a viscous brown gum, which is the triketone 2-ethyl-2-(6-m-methoxyphenyl-5-methyl-3-oxohexyl)cyclopentane-1,3-dione.

WORKUP

后处理

  1. additionAdd
  2. temperatureheat the mixture
  3. temperatureunder reflux for 6 hours
  4. customRemove most of the solvent under reduced pressure
  5. additionadd ether (25 cc) and benzene (25 cc) to the residue
  6. washWash the solution with 5% aqueous sodium hydroxide, water, dilute hydrochloric acid, and brine
  7. customdry
  8. customEvaporate the solvent
  9. customto obtain a viscous brown gum, which