HRID2257908

反应详情

EQUATION

反应方程式

HRID 2257908 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 13.7 g of 6-[3-(N-cyclohexyl-N-methylaminocarbonyl)propoxy]carbostyril and 4.45 g of phosphorus pentasulfide in 200 ml of benzene was refluxed for 5 hours. The reaction mixture was allowed to cool. The insolubles were removed by filtration. The filtrate was subjected to distillation to remove the solvent. The resulting residue was purified by a silica gel column chromatography (eluant: 5% methanol/dichloromethane) to obtain 7.2 g of 6-[3-(N-cyclohexyl-N-methylaminothio-carbonyl)propoxy]carbostyril.

WORKUP

后处理

  1. temperatureto cool
  2. customThe insolubles were removed by filtration
  3. distillationThe filtrate was subjected to distillation
  4. customto remove the solvent
  5. customThe resulting residue was purified by a silica gel column chromatography (eluant: 5% methanol/dichloromethane)