HRID1699445
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
14.7 g (0.1 mol) of 5-aminotetralin were refluxed with 18 g (0.11 mol) of bis(β-chloroethyl)amine hydrochloride in 300 ml of n-butanol for 48 h and, after cooling, 5.4 g of sodium carbonate were added and the mixture was refluxed for a further 20 h. The precipitate which formed on cooling was filtered off with suction and taken up in water, and 2N sodium hydroxide solution was added. The aqueous phase was extracted with ethyl acetate, and washing with water and drying over sodium sulfate were followed by evaporation under reduced pressure. It was possible in this way to isolate 10.7 g (50%) of the product as an oil.
WORKUP
后处理
- temperatureafter cooling
- temperaturethe mixture was refluxed for a further 20 h
- customThe precipitate which formed
- temperatureon cooling
- filtrationwas filtered off with suction
- addition2N sodium hydroxide solution was added
- extractionThe aqueous phase was extracted with ethyl acetate
- washwashing with water
- dry with materialdrying over sodium sulfate
- customwere followed by evaporation under reduced pressure