Reaktion #3940

Reaktionsgleichung

1-bromo-3-chloropropane

1-(4-chlorobenzyl)homopiperazine

potassium hydroxide

→

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

Ausbeute 42.0%

Lösungsmittel

dimethyl sulfoxide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigean additional 30 minutes
2. 2
   Sonstigeat room temperature
3. 3
   Extraktionthe product was extracted with ether
4. 4
   Trocknenthe extract was dried (magnesium sulfate)
5. 5
   Einengenconcentrated in vacuo
6. 6
   SonstigeFinal purification
7. 7
   Sonstigethe solvent was removed in vacuo

Vorschrift

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.

Quelle