HRID1657432

反应详情

EQUATION

反应方程式

HRID 1657432 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2.46 g. of 1-(p-chlorophenylsulfinyl)-3-chloropropane, 0.9 g. of piperidine, 0.53 g. of sodium carbonate in 30 ml. of dimethylformamide is heated for 3 hours at a temperature of 80° - 87°C. After the reaction mixture has been cooled, a mixture of benzene and water is added thereto. The aqueous layer is separated and extracted with benzene. The organic layers are combined, washed with water, dried over sodium sulfate and evaporated under reduced pressure. The oily residue is dissolved in ether and treated with ethanolic hydrogen chloride under cooling. The precipitate is collected by filtration and dried to give 1-[γ-(p-chlorophenylsulfinyl)-propyl]piperidine hydrochloride, m.p.: 170° - 174°C. Recrystallization from benzene gives white crystals, m.p.: 176° - 177°C.

WORKUP

后处理

  1. additionA mixture of 2.46 g
  2. temperatureAfter the reaction mixture has been cooled
  3. additionis added
  4. customThe aqueous layer is separated
  5. extractionextracted with benzene
  6. washwashed with water
  7. dry with materialdried over sodium sulfate
  8. customevaporated under reduced pressure
  9. dissolutionThe oily residue is dissolved in ether
  10. additiontreated with ethanolic hydrogen chloride
  11. temperatureunder cooling
  12. filtrationThe precipitate is collected by filtration
  13. customdried