HRID1614626

反应详情

EQUATION

反应方程式

HRID 1614626 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3.41 g (11.3 mmol) of the N,α-bis(4-fluorophenyl)-4-piperidinemethanamine and 2.20 g (14.7 mmol) of 1,2-epoxy-3-phenoxypropane in 400 mL of acetonitrile was heated at reflux for 46 h. The solvent was removed in vacuo, and the residue was subjected to flash chromatography (silica gel, eluted with 3% CH3OH in CH2Cl2) to give an oil. This was converted to the HCl salt, and the salt was recrystallized from CH3OH-ether to give give 3.20 g (53%) of a crystalline white solid, mp 229°-232° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 46 h
  3. customThe solvent was removed in vacuo
  4. washthe residue was subjected to flash chromatography (silica gel, eluted with 3% CH3OH in CH2Cl2)
  5. customto give an oil
  6. customthe salt was recrystallized from CH3OH-ether
  7. customto give