HRID969735

反应详情

EQUATION

反应方程式

HRID 969735 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 29.2 g (0.1116 mole) of 4-(2,4-difluoro-benzoyl)-piperidine-hydrochloride, 25.3 g (0.1117 mole) of 3-(2-chloroethyl)-6,7,8,9-tetrahydro-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one, 500 ml of acetonitrile, 19.6 g (0.2333 mole) of sodium hydrogencarbonate and 0.25 g (0.0015 mole) of potassium iodide is heated to boiling for 10 hours with stirring. The reaction mixture is cooled to room temperature, to the residue 200 ml of water are added. The mixture is stirred for 30 minutes and extracted with 200 ml of dichloromethane. The organic phase is separated, dried over magnesium sulfate, filtered and the filtrate is evaporated. The oily residue thus obtained is purified as follows:

WORKUP

后处理

  1. temperatureis heated
  2. additionare added
  3. stirringThe mixture is stirred for 30 minutes
  4. extractionextracted with 200 ml of dichloromethane
  5. customThe organic phase is separated
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. customthe filtrate is evaporated
  9. customThe oily residue thus obtained
  10. customis purified