HRID2260590

反应详情

EQUATION

反应方程式

HRID 2260590 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

After 1.09 g of Compound 4 obtained in Example 4 was dissolved in 10 ml of toluene, 1.07 g of Lawesson's reagent was added to the solution. The mixture was heated under reflux for an hour. The reaction mixture was allowed to stand at room temperature, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography [eluent: hexane-ethyl acetate (2:1)] to obtain 1.46 g of a crude product. The crude product was recrystallized from ethyl acetate-hexane to obtain 1.09 g of Compound 36.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for an hour
  3. customto stand at room temperature
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography [eluent: hexane-ethyl acetate (2:1)]
  6. customto obtain 1.46 g of a crude product
  7. customThe crude product was recrystallized from ethyl acetate-hexane