Ethyl trichloroacetate → N-methyl-4-(4-(2,2,2-trichloroacetamido)phenoxy)picolinamide

HRID 2094784

Reaktionsgleichung

Reaktionsgleichung von HRID 2094784
[NH2:1][C:2]1[CH:18]=[CH:17][C:5]([O:6][C:7]2[CH:12]=[CH:11][N:10]=[C:9]([C:13]([NH:15][CH3:16])=[O:14])[CH:8]=2)=[CH:4][CH:3]=1.C([O:21][C:22](=O)[C:23]([Cl:26])([Cl:25])[Cl:24])C>C1(C)C=CC=CC=1>[CH3:16][NH:15][C:13](=[O:14])[C:9]1[CH:8]=[C:7]([O:6][C:5]2[CH:17]=[CH:18][C:2]([NH:1][C:22](=[O:21])[C:23]([Cl:26])([Cl:25])[Cl:24])=[CH:3][CH:4]=2)[CH:12]=[CH:11][N:10]=1

Komponenten

4

Edukt 2

HCID 10588Ethyl trichloroacetateHCID 166551294-(4-Aminophenoxy)-N-methylpicolinamide

Produkt 1

HCID 68728447N-methyl-4-(4-(2,2,2-trichloroacetamido)phenoxy)picolinamideAusbeute 87,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

4-(4-aminophenoxy)-N-methylpicolinamide (35 g, 0.144 mol) was mixed with ethyl-2,2,2-trichloroacetate (50 ml, 0.27 mol) in toluene (350 ml) at ambient temperature. The mixture was then heated to 100° C. under distillation mode for 2-3 hours. The organic solvent was degassed under reduced pressure to obtain oil. This oil was triturated with hexane (500 ml) to obtain (49 g) of the desired solid.

Aufarbeitung

  1. customThe organic solvent was degassed under reduced pressure
  2. customto obtain oil
  3. customThis oil was triturated with hexane (500 ml)

Quellen und Nachweise

ORD-Eintrag
ord-284905d4c53f4ad3bcd9f9c896f6b010
Quelldatensatz
uspto-grants-2013_05
Patentnummer
US08445687B2

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