HRID1707285

反应详情

EQUATION

反应方程式

HRID 1707285 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.6 g (16 mmol) 3-(6-chlorohexanoyl)-1,4,5,6,7,8,-hexahydro-2-methyl-4-(3-nitrophenyl) 5-oxo-quinoline and 9 g( 32 mmol) 4,4-diphenylpiperidine hydrochloride are boiled under reflux with 2.5 g (16 mmol) sodium iodide and 7 g (66 mmol) sodium carbonate in 150 ml acetone for 6 days. The mixture is filtered and concentrated, and the residue is taken up in 150 ml ethyl acetate. The mixture is extracted by shaking with 40 ml sodium thiosulphate solution (5%). The organic phase is dried over magnesium sulphate, filtered and concentrated. The residue is chromatographed over silica gel with toluene/acetone=8/2. The title compound is obtained as a yellow oil. Yield: 8 g (82%).

WORKUP

后处理

  1. filtrationThe mixture is filtered
  2. concentrationconcentrated
  3. extractionThe mixture is extracted
  4. dry with materialThe organic phase is dried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue is chromatographed over silica gel with toluene/acetone=8/2