HRID1165286

反应详情

EQUATION

反应方程式

HRID 1165286 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under inert atmosphere, 1 g of 1-methyl-quinolin-2-one and 25 ml of benzene were mixed together and then 1.27 g of 2,4-bis-(4-methoxyphenyl)-2,4-dithioxo-1,3,2,4-dithiadiphos phetane (Laweseeon's reagent) were added all at once. After stirring at reflux for 1 hour, cooling, eliminating the solvent by distilling under reduced pressure and drying under a good vacuum and chromatographing, the residue was chromatographed on silica and eluted with a mixture of methylene chloride and ethyl acetate (1/1) to obtain 1 g of the product sought melting at 114° C.

WORKUP

后处理

  1. temperatureat reflux for 1 hour
  2. temperaturecooling
  3. distillationby distilling under reduced pressure
  4. customdrying under a good vacuum and chromatographing
  5. customthe residue was chromatographed on silica
  6. washeluted with a mixture of methylene chloride and ethyl acetate (1/1)