반응 #3940

반응 방정식

1-bromo-3-chloropropane

1-(4-chlorobenzyl)homopiperazine

potassium hydroxide

→

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

수율 42.0%

용매

dimethyl sulfoxide

반응 조건

후처리

1. 1
   기타an additional 30 minutes
2. 2
   기타at room temperature
3. 3
   추출the product was extracted with ether
4. 4
   건조the extract was dried (magnesium sulfate)
5. 5
   농축concentrated in vacuo
6. 6
   기타Final purification
7. 7
   기타the solvent was removed in vacuo

실험 절차

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.

출처