反応 #3941

反応方程式

sodium hydroxide

thiourea

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

ethanol

→

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

収率 39.1%

溶媒

water

反応条件

後処理

1. 1
   温度The mixture was refluxed for 6 hours
2. 2
   温度the resulting solution was refluxed for 4 hours
3. 3
   その他The ethanol was removed in vacuo, and water
4. 4
   workup.ADDITIONwas added to the residue
5. 5
   抽出The product was extracted with methylene chloride
6. 6
   乾燥the extract was dried (sodium sulfate)
7. 7
   濃縮concentrated

実験手順

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.

出典