Reaktion #3886

Reaktionsgleichung

thiourea

benzyl-4-(3-chloropropyl)piperazine dihydrochloride

triethylamine

sodium hydroxide

→

3-(4-benzylpiperazin-1-yl)propanethiol dihydrochloride

Ausbeute 78.0%

Lösungsmittel

ethanol

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was refluxed for 8 hours
2. 2
   Temperaturthe resulting mixture was refluxed for 4 additional hours
3. 3
   SonstigeThe ethanol was removed in vacuo, and water
4. 4
   workup.ADDITIONadded to the residue which
5. 5
   Extraktionwas extracted with methylene chloride
6. 6
   Trocknendried (sodium sulfate)
7. 7
   Sonstigethe salt was precipitated with ethereal hydrochloric acid

Vorschrift

15 g of thiourea were added to a solution of 35 g of -benzyl-4-(3-chloropropyl)piperazine dihydrochloride, 20 g of triethylamine and 250 ml of reagent ethanol, and the mixture was refluxed for 8 hours. After the addition of a solution of 10 g of sodium hydroxide in 50 ml of water, the resulting mixture was refluxed for 4 additional hours. The ethanol was removed in vacuo, and water added to the residue which was extracted with methylene chloride, dried (sodium sulfate), and the salt was precipitated with ethereal hydrochloric acid to give 25.1 g (78% of theory) of 3-(4-benzylpiperazin-1-yl)propanethiol dihydrochloride as a white crystalline solid, M.p. 270°-273° C. (dec.).

Quelle