Reaktion #3941

Reaktionsgleichung

sodium hydroxide

thiourea

1-(4-chlorobenzyl)-4-(3-chloropropyl)homopiperazine

ethanol

→

3-[4-(4-chlorobenzyl)homopiperazin-1-yl]propanethiol

Ausbeute 39.1%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was refluxed for 6 hours
2. 2
   Temperaturthe resulting solution was refluxed for 4 hours
3. 3
   SonstigeThe ethanol was removed in vacuo, and water
4. 4
   workup.ADDITIONwas added to the residue
5. 5
   ExtraktionThe product was extracted with methylene chloride
6. 6
   Trocknenthe extract was dried (sodium sulfate)
7. 7
   Einengenconcentrated

Vorschrift

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.

Quelle