Reacción #3928

ord-b5880115943c4665b571bee98c011ee9

Ecuación de reacción

Clc1ccc(CN2CCNCC2)cc1
1-(4-chlorobenzyl)piperazine
ClCCBr
1-bromo-2-chloroethane
Cl.Cl.ClCCN1CCN(Cc2ccc(Cl)cc2)CC1
1-(4-chlorobenzyl)-4-(2-chloroethyl)piperazine dihydrochloride
Rendimiento 112.0%

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawas refluxed for 8 hours
  2. 2
    OtroThe solvent was removed in vacuo, and 2N sodium hydroxide
  3. 3
    workup.ADDITIONwas added to the residue
  4. 4
    ExtracciónThe product was extracted with methylene chloride
  5. 5
    Secadothe extract was dried (sodium sulfate)
  6. 6
    Concentraciónconcentrated
  7. 7
    OtroThe salt was precipitated with ethereal hydrochloric acid

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04722926uspto-grants-1988_02