反応 #3886

反応方程式

thiourea

benzyl-4-(3-chloropropyl)piperazine dihydrochloride

triethylamine

sodium hydroxide

→

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

収率 78.0%

溶媒

ethanol

water

反応条件

後処理

1. 1
   温度the mixture was refluxed for 8 hours
2. 2
   温度the resulting mixture was refluxed for 4 additional hours
3. 3
   その他The ethanol was removed in vacuo, and water
4. 4
   workup.ADDITIONadded to the residue which
5. 5
   抽出was extracted with methylene chloride
6. 6
   乾燥dried (sodium sulfate)
7. 7
   その他the salt was precipitated with ethereal hydrochloric acid

実験手順

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.).

出典