반응 #3886

반응 방정식

thiourea

benzyl-4-(3-chloropropyl)piperazine dihydrochloride

triethylamine

sodium hydroxide

→

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

수율 78.0%

용매

ethanol

water

반응 조건

후처리

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

실험 절차

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.).

출처