HRID609565

反应详情

EQUATION

反应方程式

HRID 609565 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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 4 hours. 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

  1. temperature0.008 moles, and the reaction was heated
  2. temperatureto reflux for 4 hours
  3. customthe solvent was decanted
  4. additionTo the residue was added 25 ml of isopropanol and 150 ml of ethyl acetate
  5. customA solid crystallized
  6. filtrationwas collected by filtration
  7. customThe above solid was then dried at 80° C. for 24 hours