HRID1433108

反应详情

EQUATION

反应方程式

HRID 1433108 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4.2 g of 2-methyl-1-[4-fluorophenyl]-2-morpholinopropan-1-one (0.0167 moles), 5.75 g of piperazine (0.0669 moles), 0.063 g of copper (I) iodide and 15 ml of toluene were mixed in a three necked flask equipped with a stirrer, nitrogen inlet, condenser, nitrogen outlet and a temperature probe. The mixture was heated to reflux for a total of 24 hours under a constant flow of nitrogen gas. The mixture was then cooled to room temperature, after which it was dissolved in 75 ml of dichloromethane. The mixture was then extracted with 100 ml of a saturated aqueous sodium chloride solution and then with 2×100 ml of water. The dichloromethane layer was then dried using anhydrous magnesium sulphate. The magnesium sulphate was removed by filtration and the organic solvent was then removed on a rotary evaporator to yield the product.

WORKUP

后处理

  1. customequipped with a stirrer, nitrogen inlet, condenser, nitrogen outlet
  2. temperatureThe mixture was heated
  3. temperatureto reflux for a total of 24 hours under a constant flow of nitrogen gas
  4. extractionThe mixture was then extracted with 100 ml of a saturated aqueous sodium chloride solution
  5. dry with materialThe dichloromethane layer was then dried
  6. customThe magnesium sulphate was removed by filtration
  7. customthe organic solvent was then removed on a rotary evaporator
  8. customto yield the product