HRID1087116

反应详情

EQUATION

反应方程式

HRID 1087116 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.5 g 2-(3- chloropropylthio)benzamide, 5.3 g of 4-[3-(ethylamino) -2-hydroxypropoxy]- benzonitrile, 6.6 g potassium carbonate and 7.2 g sodiumiodide were mixed in 100 ml of acetonitrile and heated to reflux for two days. The mixture was filtered and evaporated and the residue was dissolved in 1 M sulphuric acid. The acidic water layer was then washed twice with ether, alkalized with 10 M sodiumhydroxide and extracted with dichlormethane. The organic layer was dried over sodiumsulphate, treated with active carbon, filtered and evaporated. The residue, 8.7 g, was separated by column chromatography. Yield: 4.5 g of the title compound.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for two days
  3. filtrationThe mixture was filtered
  4. customevaporated
  5. dissolutionthe residue was dissolved in 1 M sulphuric acid
  6. washThe acidic water layer was then washed twice with ether
  7. extractionextracted with dichlormethane
  8. dry with materialThe organic layer was dried over sodiumsulphate
  9. additiontreated with active carbon
  10. filtrationfiltered
  11. customevaporated
  12. customThe residue, 8.7 g, was separated by column chromatography