Reaktion #3928
ord-b5880115943c4665b571bee98c011ee9
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturwas refluxed for 8 hours
- 2SonstigeThe solvent was removed in vacuo, and 2N sodium hydroxide
- 3workup.ADDITIONwas added to the residue
- 4ExtraktionThe product was extracted with methylene chloride
- 5Trocknenthe extract was dried (sodium sulfate)
- 6Einengenconcentrated
- 7SonstigeThe salt was precipitated with ethereal hydrochloric acid
Vorschrift
A mixture of 15.0 g of 1-(4-chlorobenzyl)piperazine, 14.4 g of 1-bromo-2-chloroethane and 150 ml of tetrahydrofuran was refluxed for 8 hours. The solvent was removed in vacuo, and 2N sodium hydroxide was added to the residue. The product was extracted with methylene chloride, and the extract was dried (sodium sulfate) and concentrated. The salt was precipitated with ethereal hydrochloric acid to give 13.8 g (56% of theory) of 1-(4-chlorobenzyl)-4-(2-chloroethyl)piperazine dihydrochloride as a white crystalline solid.