HRID1681079

反应详情

EQUATION

反应方程式

HRID 1681079 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A reaction mixture containing phenyl(4-piperidinyl)methanone (20.5 g, 0.108 mol), K2CO3 (33.17 g, 0.18 mol), potassium iodide (0.2 g) and 2-bromoethyl benzene (22.2 g, 0.12 mol, 16.4 ml) in toluene (250 ml) was stirred at reflux temperature for 66 h. The reaction mixture was filtered and the filtrate concentrated to a residue which was dissolved in dry Et2O (500 ml) and treated dropwise with a solution of HCl (0.11 mol) in EtOAc. The resultant precipitate was recrystallized from EtOH:CH3OH, 4:1 (500 ml) to give phenyl[1-(2-phenylethyl)-4-piperidinyl]-methanone hydrochloride, mp 258°-260° C.

WORKUP

后处理

  1. temperatureat reflux temperature for 66 h
  2. filtrationThe reaction mixture was filtered
  3. concentrationthe filtrate concentrated to a residue which
  4. dissolutionwas dissolved in dry Et2O (500 ml)
  5. customThe resultant precipitate was recrystallized from EtOH