Reaktion #318559

ord-4e26d05449f846529a1c30fbcf8ff566

Reaktionsgleichung

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

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturis heated
  2. 2
    Temperaturto reflux of the dioxon
  3. 3
    SonstigeThe product expected crystallizes
  4. 4
    Waschenwashing with water
  5. 5
    Sonstigedrying
  6. 6
    Temperaturby heating under vacuum
  7. 7
    Sonstigethe product is recrystallized from acetonitrile

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04845293uspto-grants-1989_07