تفاعل #3941

ord-73e545c91cc447a8af0c692a3811aa45

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was refluxed for 6 hours
  2. 2
    درجة الحرارةthe resulting solution was refluxed for 4 hours
  3. 3
    أخرىThe ethanol was removed in vacuo, and water
  4. 4
    workup.ADDITIONwas added to the residue
  5. 5
    استخلاصThe product was extracted with methylene chloride
  6. 6
    تجفيفthe extract was dried (sodium sulfate)
  7. 7
    تركيزconcentrated

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04722926uspto-grants-1988_02