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
26.6 g (0.1 mole) of diethyl phenethylmalonate were added dropwise in the course of an hour, with stirring, to 5.6 g of KOH in 65 ml of absolute ethanol, the mixture was stirred at room temperature for 15 hours and then boiled for 5 minutes. The ethanol was removed in vacuo, ice-water was added and the mixture was extracted with ether. The aqueous phase was acidified with 2N hydrochloric acid and extracted with ether. The second extract was dried and evaporated and then neutralized with 8.8 ml of diethylamine. 12 ml of 30% strength formaldehyde solution were added, the mixture was stirred for 3 hours, then saturated with potassium carbonate, extracted with ether, the extract was washed with dilute hydrochloric acid, dried and evaporated.
WORKUP
后处理
- waitboiled for 5 minutes
- customThe ethanol was removed in vacuo, ice-water
- additionwas added
- extractionthe mixture was extracted with ether
- extractionextracted with ether
- extractionThe second extract
- customwas dried
- customevaporated
- addition12 ml of 30% strength formaldehyde solution were added
- stirringthe mixture was stirred for 3 hours
- extractionsaturated with potassium carbonate, extracted with ether
- washthe extract was washed with dilute hydrochloric acid
- customdried
- customevaporated