HRID1607760
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheated at 70°-80° C. for 5 hours
- customThe DMF is removed under reduced pressure
- dissolutionthe residue is dissolved in chloroform
- washthe chloroform solution is washed with water (2×), 1N KOH (2×), 1N HCl, and water again (3×)
- dry with materialThe washed chloroform solution is dried
- customsolvent is removed
- customto give an oil which
- customis evaporated twice with chloroform/ether
- customto give a solid
- customRecrystallization from ether (500 ml)