HRID2187544

反应详情

EQUATION

反应方程式

HRID 2187544 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-[4-(2-pyridyl)piperidin-1-yl]propylamine, (6), (637.9 g, 3.86 mol) in ethanol (8.5 L) was warmed to 65° C. A solution of L-tartaric acid (637.9 g, 4.25 mol) in ethanol (2.23 L) was added in portions. Approximately 15% of the tartaric acid solution was added and then reaction mixture was aged for 1 hour to afford a thin slurry of crystalline material. The remaining tartaric acid solution was added dropwise. Heating was discontinued and the solution was slowly cooled to ambient temperature overnight. The solids were filtered, rinsed with ethanol (2×1 L) and dried under a stream of nitrogen to afford 3-[4-(2-pyridyl)piperidin-1-yl]propylamine L-tartrate salt, (7), as a pale yellow solid.

WORKUP

后处理

  1. customreaction mixture
  2. customto afford a thin slurry of crystalline material
  3. temperatureHeating
  4. filtrationThe solids were filtered
  5. washrinsed with ethanol (2×1 L)
  6. customdried under a stream of nitrogen