HRID279293

反应详情

EQUATION

反应方程式

HRID 279293 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of 4-(aminomethyl)piperidine (7.00 g, 61.3 mmol) in CH3CN (100 mL) was treated sequentially with K2CO3 (3.02 g) and 4-chlorobenzyl chloride (3.52 g, 21.8 mmol). The reaction mixture was heated to 60° C. for 16 h, cooled to 25° C. and concentrated. The residue was partitioned between CH2Cl2 (75 mL) and water (50 mL), and was washed with water (2×50 mL) and brine (1×50 mL). The organic phase was dried (MgSO4) and concentrated. Chromatography (SiO2, 4% H2O-iPrOH) afforded4-(aminomethyl)-1-(4-chlorobenzyl)piperidine (3.58 g, 69%).

WORKUP

后处理

  1. temperaturecooled to 25° C.
  2. concentrationconcentrated
  3. customThe residue was partitioned between CH2Cl2 (75 mL) and water (50 mL)
  4. washwas washed with water (2×50 mL) and brine (1×50 mL)
  5. dry with materialThe organic phase was dried (MgSO4)
  6. concentrationconcentrated