HRID1391471

反应详情

EQUATION

反应方程式

HRID 1391471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1 g of potassium hydroxide is dissolved in 40 ml of methanol and mixed with 2.3 g of 4-nitrothiophenol. The suspension is stirred for one hour at room temperature and mixed drop by drop with 1.48 ml of 1-bromo-3-chloropropane. After 4 hours of stirring at room temperature, another 0.15 ml of 1-bromo-3-chloropropane is added in drops. The mixture is stirred for 65 hours at room temperature, concentrated by evaporation in a vacuum and taken up in ethyl acetate. It is extracted with water and saturated common salt solution, dried on sodium sulfate and concentrated by evaporation. After purification by flash chromatography, 2.54 g of 1-(3-chloro-propylsulfanyl)-4-nitro-benzene is obtained.

WORKUP

后处理

  1. stirringAfter 4 hours of stirring at room temperature
  2. stirringThe mixture is stirred for 65 hours at room temperature
  3. concentrationconcentrated by evaporation in a vacuum
  4. extractionIt is extracted with water and saturated common salt solution
  5. customdried on sodium sulfate
  6. concentrationconcentrated by evaporation
  7. customAfter purification by flash chromatography