Reacción #321871

ord-1a40979f43e34f1ab5ba335d8b58d90b

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Extracciónextracted three times with 50 ml of ethyl acetate each time
  2. 2
    LavadoThe combined extracts were washed with a small amount of water
  3. 3
    Concentraciónconcentrated
  4. 4
    OtroThe residue was recrystallized from 80 ml of acetone

Procedimiento

2.5 g of N-(2-chloroethyl)-7-chloro-4-quinolinamine hydrochloride in 25 ml of 3-methylpiperidine were held at 100° C. in a sealed tube for 24 hours. Thereafter, 100 ml of water were added, the mixture is adjusted to pH 12 by means of concentrated sodium hydroxide solution and extracted three times with 50 ml of ethyl acetate each time. The combined extracts were washed with a small amount of water and concentrated. The residue was recrystallized from 80 ml of acetone. 0.88 g of colourless crystals, m.p.: 148°-151° C., was obtained.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05596002uspto-grants-1997_01