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
A solution of 3.12 g. (0.02 mole) of 2-(2-dimethylaminoethyl)piperidine and 4.8 g. (0.02 mole) of 9-acetoxyxanthene in 75 ml. of anhydrous benzene was refluxed for 20 hours. The cooled solution was washed with 100 ml. of a 5 percent aqueous sodium bicarbonate solution, dried over anhydrous potassium carbonate, filtered, and evaporated in vacuo. The residue was taken up in low boiling petroleum ether and filtered to remove dixanthenyl ether. The filtrate was chromatographed on 125 g. of alumina, eluting successively with petroleum ether, petroleum etherbenzene mixtures, benzene, and finally ether. Evaporation of the ether fractions gave 1-(9-xanthenyl)-2-(2-dimethylaminoethyl)piperidine, m.p. 64°-67°C.
WORKUP
后处理
- washThe cooled solution was washed with 100 ml
- dry with materialof a 5 percent aqueous sodium bicarbonate solution, dried over anhydrous potassium carbonate
- filtrationfiltered
- customevaporated in vacuo
- filtrationfiltered
- customto remove dixanthenyl ether
- customThe filtrate was chromatographed on 125 g
- washof alumina, eluting successively with petroleum ether, petroleum etherbenzene mixtures, benzene, and finally ether
- customEvaporation of the ether fractions