HRID1607760

反应详情

EQUATION

反应方程式

HRID 1607760 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-fluoromethyl-2-phthalimido-5-iodopentanenitrile (34.1 g), potassium phthalimide (16.6 g), and dry DMF (230 ml) is stirred and heated at 70°-80° C. for 5 hours. The DMF is removed under reduced pressure, the residue is dissolved in chloroform, and the chloroform solution is washed with water (2×), 1N KOH (2×), 1N HCl, and water again (3×). The washed chloroform solution is dried and solvent is removed to give an oil which is evaporated twice with chloroform/ether to give a solid. Recrystallization from ether (500 ml) gives pure 2-fluoromethyl-2,5-diphthalimidopentanenitrile (18.5 g).

WORKUP

后处理

  1. temperatureheated at 70°-80° C. for 5 hours
  2. customThe DMF is removed under reduced pressure
  3. dissolutionthe residue is dissolved in chloroform
  4. washthe chloroform solution is washed with water (2×), 1N KOH (2×), 1N HCl, and water again (3×)
  5. dry with materialThe washed chloroform solution is dried
  6. customsolvent is removed
  7. customto give an oil which
  8. customis evaporated twice with chloroform/ether
  9. customto give a solid
  10. customRecrystallization from ether (500 ml)