HRID330281

反应详情

EQUATION

反应方程式

HRID 330281 的结构方程式

PROCEDURE

实验过程

According to the procedure of W. K. Anderson et al., J. Chem. Soc., Perkin 1, 1 (1976) a mixture of 4-bromothiophenol (40.0 g, 0.211 mol) and K2CO3 (35.3 g, 0.254 mol) was heated at reflux for 1 hour. 2,3-Dichloro-1-propene (23.5 g, 0.211 mol) was added. The resulting mixture was heated at reflux for 2 hours, cooled and concentrated. The mixture was diluted with H2O and extracted with ether (3×150 mL). The combined extracts were dried (MgSO4), and concentrated to give an oil. Distillation under high vacuum gave 37.2 g (67%) of product as a colorless liquid.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 1 hour
  3. temperatureThe resulting mixture was heated
  4. temperatureat reflux for 2 hours
  5. temperaturecooled
  6. concentrationconcentrated
  7. additionThe mixture was diluted with H2O
  8. extractionextracted with ether (3×150 mL)
  9. dry with materialThe combined extracts were dried (MgSO4)
  10. concentrationconcentrated
  11. customto give an oil
  12. distillationDistillation under high vacuum