HRID1418848
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
To a stirred suspension of the product of step (a), 2.0 g, 0.006 moles, in 35 ml of chlorobenzene was added 4-dimethylaminopyridine. To this was added 1-pyrrolidinecarbonitrile, 1.5 ml; 0.008 moles, and the reaction was heated to reflux for 4hours. The reaction cooled to room temperature and the solvent was decanted. To the residue was added 25 ml of isopropanol and 150 ml of ethyl acetate. A solid crystallized and was collected by filtration. The above solid was then dried at 80° C. for 24 hours to give N-[3-(((4-phenylbutyl)amino)carbonyl)phenyl]-1-pyrrolidinecarboximidamide hydrochloride, 2.3 g, m.p. 197°-198° C.
WORKUP
后处理
- temperature0.008 moles, and the reaction was heated
- temperatureto reflux for 4hours
- customthe solvent was decanted
- additionTo the residue was added 25 ml of isopropanol and 150 ml of ethyl acetate
- customA solid crystallized
- filtrationwas collected by filtration
- customThe above solid was then dried at 80° C. for 24 hours