Reaktion #3937

Reaktionsgleichung

cinnamyl bromide

1-(3-chloropropyl)piperazine dihydrochloride hemihydrate

triethylamine

→

1-cinnamyl-4-(3-chloropropyl)piperazine dihydrochloride

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was refluxed for 4 hours
2. 2
   SonstigeAfter removal of the solvent in vacuo, water
3. 3
   workup.ADDITIONwas added to the residue
4. 4
   ExtraktionThe product was then extracted with ether
5. 5
   Trocknenthe extract was dried (magnesium sulfate)
6. 6
   Einengenconcentrated
7. 7
   SonstigeThe resulting oil was chromatographed on silica gel (methylene chloride/methanol: 9/1)
8. 8
   Sonstigeprecipitated with ethereal hydrochloric acid

Vorschrift

6.0 g of cinnamyl bromide were added to a mixture of 7.4 g of 1-(3-chloropropyl)piperazine dihydrochloride hemihydrate, 6.1 g of triethylamine and 100 ml of reagent ethanol. The mixture was refluxed for 4 hours and then stirred overnight. After removal of the solvent in vacuo, water was added to the residue. The product was then extracted with ether and the extract was dried (magnesium sulfate) and concentrated. The resulting oil was chromatographed on silica gel (methylene chloride/methanol: 9/1) and precipitated with ethereal hydrochloric acid to give 7.4 g (70% of theory) of 1-cinnamyl-4-(3-chloropropyl)piperazine dihydrochloride.

Quelle