反应 #3941

ord-73e545c91cc447a8af0c692a3811aa45

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The mixture was refluxed for 6 hours
  2. 2
    温度the resulting solution was refluxed for 4 hours
  3. 3
    其他The ethanol was removed in vacuo, and water
  4. 4
    workup.ADDITIONwas added to the residue
  5. 5
    萃取The product was extracted with methylene chloride
  6. 6
    干燥the extract was dried (sodium sulfate)
  7. 7
    浓缩concentrated

实验过程

4.1 g of thiourea were added to a mixture of 8.0 g of 1-(4-chlorobenzyl)-4-(3-chloropropyl)homopiperazine and 100 ml of reagent ethanol. The mixture was refluxed for 6 hours and then stirred overnight at room temperature. A solution of 5.0 g of sodium hydroxide in 30 ml of water was added, and the resulting solution was refluxed for 4 hours. The ethanol was removed in vacuo, and water was added to the residue. The product was extracted with methylene chloride, and the extract was dried (sodium sulfate) and concentrated to give 3.1 g (39% of theory) of 3-[4-(4-chlorobenzyl)homopiperazin-1-yl]propanethiol as a yellow oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04722926uspto-grants-1988_02