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 mixture of 6.5 parts 5-cyano-5-(2-bromoethyl)10,11-dihydro-5H-dibenzo[a,d]cycloheptene, 4.0 parts 2-azabicyclo[2.2.2]octane hydrochloride and 4.0 parts potassium carbonate in 88 parts N,N-dimethylsulfoxide and 20 parts water is heated at reflux for about 4 hours. After cooling, the reaction mixture is diluted with water, resulting in the formation of an oil. The water layer is decanted and the oil dissolved in ethyl ether. The ethereal solution is washed twice with water, once with a saturated sodium chloride solution, dried over anhydrous sodium sulfate and filtered. The solvent is removed to give an oil which is treated with a solution of hydrogen chloride in isopropanol. Addition of ethyl ether results in a precipitate that is separated, washed with ether and dried to afford-5-cyano-5[2-(2-azabicyclo[2.2.2]oct-2-yl)ethyl]-10,11-dihydro-5H-dibenzo[a,d]cycloheptene hydrochloride. This compound is represented by the following structural formula. ##STR14##
WORKUP
后处理
- temperatureis heated
- temperatureat reflux for about 4 hours
- temperatureAfter cooling
- customresulting in the formation of an oil
- customThe water layer is decanted
- dissolutionthe oil dissolved in ethyl ether
- washThe ethereal solution is washed twice with water, once with a saturated sodium chloride solution
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- customThe solvent is removed
- customto give an oil which
- customresults in a precipitate that
- customis separated
- washwashed with ether
- customdried