Reaktion #2159844

Reaktionsgleichung

2-(4-t-octylphenoxy)-butyric acid chloride

1-(2,4,6-trichlorophenyl)-3-(2-chloro-5-aminoanilino)-5-pyrazolone

sodium acetate

→

1-(2,4,6-trichlorophenyl)-3-[2-chloro-5-{2-(4-t-octylphenoxy)butaneamido}anilino]-5-pyrazolone

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe organic phase was separated from the reaction liquid
2. 2
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
3. 3
   SonstigeThe residuum was recrystallized from 300 ml of ethanol

Vorschrift

Forty point four grams of 1-(2,4,6-trichlorophenyl)-3-(2-chloro-5-aminoanilino)-5-pyrazolone were suspended in 120 ml of ethyl acetate, and to this mixture were added 40 ml of an aqueous solution containing 9.62 g of sodium acetate. At room temperature, 31.1 g of 2-(4-t-octylphenoxy)-butyric acid chloride were added dropwise to the liquid, and the mixture was stirred for another hour at room temperature. The organic phase was separated from the reaction liquid, and the solvent was distilled off under reduced pressure. The residuum was recrystallized from 300 ml of ethanol, whereby 58 g of objective 1-(2,4,6-trichlorophenyl)-3-[2-chloro-5-{2-(4-t-octylphenoxy)butaneamido}anilino]-5-pyrazolone were obtained. Melting point: 163° to 165° C. The structure was confirmed through the procedures of NMR, IR and MASS.

Quelle