Reacción #318559

ord-4e26d05449f846529a1c30fbcf8ff566

Ecuación de reacción

O=[N+]([O-])c1c(Cl)cc(Cl)cc1Cl
2,4,6-trichloronitrobenzene
NCCOCCO
2-(β-aminoethoxy)ethanol
O=[N+]([O-])c1c(NCCOCCO)cc(Cl)cc1NCCOCCO
4-chloro-2-(β-hydroxyethoxyethyl)amino6-(β-hydroxyethoxyethyl)aminonitrobenzene

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturais heated
  2. 2
    Temperaturato reflux of the dioxon
  3. 3
    OtroThe product expected crystallizes
  4. 4
    Lavadowashing with water
  5. 5
    Otrodrying
  6. 6
    Temperaturaby heating under vacuum
  7. 7
    Otrothe product is recrystallized from acetonitrile

Procedimiento

The mixture consisting of 0.1 mole (22.6 g) of 2,4,6-trichloronitrobenzene, 0.6 mole (63 g) of 2-(β-aminoethoxy)ethanol and 20 ml of dioxan is heated to reflux of the dioxon. After 4 hours, the reaction mixture is poured onto to 200 g of ice. The product expected crystallizes on acidifying with concentrated hydrochloric acid. After draining, washing with water and drying by heating under vacuum, the product is recrystallized from acetonitrile and then from toluene. It melts at 83° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04845293uspto-grants-1989_07