HRID1077140
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionAdd
- temperatureheat the mixture
- temperatureunder reflux for 6 hours
- customRemove most of the solvent under reduced pressure
- additionadd ether (25 cc) and benzene (25 cc) to the residue
- washWash the solution with 5% aqueous sodium hydroxide, water, dilute hydrochloric acid, and brine
- customdry
- customEvaporate the solvent
- customto obtain a viscous brown gum, which