Reaktion #3928

ord-b5880115943c4665b571bee98c011ee9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas refluxed for 8 hours
  2. 2
    SonstigeThe solvent was removed in vacuo, and 2N sodium hydroxide
  3. 3
    workup.ADDITIONwas added to the residue
  4. 4
    ExtraktionThe product was extracted with methylene chloride
  5. 5
    Trocknenthe extract was dried (sodium sulfate)
  6. 6
    Einengenconcentrated
  7. 7
    SonstigeThe 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04722926uspto-grants-1988_02