Reacción #459772

ord-d02da9a45bf74325877917a292ba46f6

Disolventes

Condiciones de reacción

Temperatura
140°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.DISTILLATIONThen, the propionic acid is distilled off under reduced pressure
  2. 2
    ExtracciónThe residue is extracted with chloroform
  3. 3
    LavadoThe chloroform layer is washed with water
  4. 4
    Secadodried over sodium sulfate
  5. 5
    OtroEvaporation of the solvent
  6. 6
    Otrogives oily residue

Procedimiento

A mixture of 0.56 part of 2-amino-3,5-dibromobenzylalcohol, 1.0 part of N-methyl piperazine and 2 parts of propionic acid is heated at 140° C for 8 hours under stirring. Then, the propionic acid is distilled off under reduced pressure. The residue is extracted with chloroform. The chloroform layer is washed with water and dried over sodium sulfate. Evaporation of the solvent gives oily residue. The residue is chromotographed over silica gel. Ethyl acetate eluates are treated with ethanolic hydrochloric acid. This procedure gives N1 -methyl-N4 -(2-amino-3,5-dibromobenzyl)piperazine hydrochloride melting at 182° to 185° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04091220uspto-grants-1978_05