反応 #3940

反応方程式

1-bromo-3-chloropropane

1-(4-chlorobenzyl)homopiperazine

potassium hydroxide

→

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

収率 42.0%

溶媒

dimethyl sulfoxide

反応条件

後処理

1. 1
   その他an additional 30 minutes
2. 2
   その他at room temperature
3. 3
   抽出the product was extracted with ether
4. 4
   乾燥the extract was dried (magnesium sulfate)
5. 5
   濃縮concentrated in vacuo
6. 6
   その他Final purification
7. 7
   その他the solvent was removed in vacuo

実験手順

15.7 g of 1-bromo-3-chloropropane were added to a cooled solution of 15.0 g of 1-(4-chlorobenzyl)homopiperazine and 12.0 g of potassium hydroxide in 50 ml of dimethyl sulfoxide. The mixture was stirred at 5°-10° C. for one hour, and then an additional 30 minutes at room temperature. After the addition of ice water, the product was extracted with ether, and the extract was dried (magnesium sulfate) and concentrated in vacuo. Final purification was effected on a silica gel column (methylene chloride:methanol, 9:1), and the solvent was removed in vacuo to give 8.4 g (42% of theory) of 1-(4-chlorobenzyl)-4-(3-chloropropyl)homopiperazine as an oil.

出典