(2,4,6-Trichlorophenyl)hydrazine → alpha-cyano-beta-(2,4,6-trichlorophenylhydrazino)-N-ethoxycarbonylacrylamide

HRID 648158

Reaktionsgleichung

Reaktionsgleichung von HRID 648158
[C:1]([C:3](=[CH:12]OCC)[C:4]([NH:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5])#[N:2].[Cl:16][C:17]1[CH:22]=[C:21]([Cl:23])[CH:20]=[C:19]([Cl:24])[C:18]=1[NH:25][NH2:26]>C(O)C.C1(C)C=CC=CC=1>[C:1]([C:3](=[CH:12][NH:26][NH:25][C:18]1[C:17]([Cl:16])=[CH:22][C:21]([Cl:23])=[CH:20][C:19]=1[Cl:24])[C:4]([NH:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5])#[N:2]

Komponenten

4

Edukt 2

HCID 79234(2,4,6-Trichlorophenyl)hydrazineHCID 230015ethyl N-(2-cyano-3-ethoxyacryloyl)carbamate

Produkt 1

HCID 70512904alpha-cyano-beta-(2,4,6-trichlorophenylhydrazino)-N-ethoxycarbonylacrylamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21863594Toluene ethanolLösungsmittel

Versuchsvorschrift

Four grams (18.9 mmol) of α-cyano-β-ethoxy-N-ethoxycarbonylacrylamide is dissolved in hot ethanol/toluene. To this is added, portionwise, 4 g of 2,4,6-trichlorophenylhydrazine. The mixture is heated to reflux for three days. Cooling of the mixture and evaporation of the solvent gives the crude product, which is recrystallized from ethanol (3 X) to yield α-cyano-β-(2,4,6-trichlorophenylhydrazino)-N-ethoxycarbonylacrylamide, m.p. =161° (dec.).

Aufarbeitung

  1. additionTo this is added
  2. temperatureThe mixture is heated
  3. temperatureto reflux for three days
  4. temperatureCooling of the mixture and evaporation of the solvent
  5. customgives the crude product, which
  6. customis recrystallized from ethanol (3 X)

Quellen und Nachweise

ORD-Eintrag
ord-d1b32aaa250e4dd1bff5836cad3b6aa9
Quelldatensatz
uspto-grants-1983_10
Patentnummer
US04411839

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