반응 #3941

ord-73e545c91cc447a8af0c692a3811aa45

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was refluxed for 6 hours
  2. 2
    온도the resulting solution was refluxed for 4 hours
  3. 3
    기타The ethanol was removed in vacuo, and water
  4. 4
    workup.ADDITIONwas added to the residue
  5. 5
    추출The product was extracted with methylene chloride
  6. 6
    건조the extract was dried (sodium sulfate)
  7. 7
    농축concentrated

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04722926uspto-grants-1988_02