HRID1607759

反应详情

EQUATION

反应方程式

HRID 1607759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-fluoromethyl-2-phthalimido-5-methanesulfonyloxypentanenitrile (42 g) and sodium iodide (35.7 g) in acetone (600 ml) is stirred and heated under reflux. After about 1/2 hour, the mixture solidifies. Acetone (500 ml) is added, and refluxing and stirring is continued overnight. The salts are removed by filtration and washed several times with acetone. The acetone is evaporated to give a residue which is dissolved in ether (1.5 l). The ether solution is washed subsequently with water (2×), sodium sulfite solution, and water again (3×). After drying (MgSO4) and evaporating the ether, 2-fluoromethyl-2-phthalimido-5-iodopentanenitrile is obtained as an oil (34.1 g).

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux
  3. temperaturerefluxing
  4. waitis continued overnight
  5. customThe salts are removed by filtration
  6. washwashed several times with acetone
  7. customThe acetone is evaporated
  8. customto give a residue which
  9. washThe ether solution is washed subsequently with water (2×), sodium sulfite solution, and water again (3×)
  10. dry with materialAfter drying (MgSO4)
  11. customevaporating the ether