1-Methylthio-1-methylamino-2-nitroethylene → HCID 70019858, Verbindung

HRID 1280393Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1280393
[CH3:1][NH:2][C:3](SC)=[CH:4][N+:5]([O-:7])=[O:6].[CH3:10][N:11]([C:13]1[C:18]([Cl:19])=[CH:17][C:16]([C:20]([F:23])([F:22])[F:21])=[CH:15][N:14]=1)[NH2:12]>O1CCOCC1>[CH3:1][NH:2][C:3]([NH:12][N:11]([CH3:10])[C:13]1[C:18]([Cl:19])=[CH:17][C:16]([C:20]([F:22])([F:21])[F:23])=[CH:15][N:14]=1)=[CH:4][N+:5]([O-:7])=[O:6]

Komponenten

4

Edukt 2

HCID 1235491-Methylthio-1-methylamino-2-nitroethyleneHCID 27367033-Chloro-2-(1-methylhydrazinyl)-5-(trifluoromethyl)pyridine

Produkt 1

HCID 70019858HCID 70019858, VerbindungAusbeute 33,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

500 mg of N-methyl-1-methylthio-2-nitroetheneamine, 770 mg of 1-methyl-1-(3-chloro-5-trifluoromethyl-2-pyridyl)hydrazine and 7 ml of 1,4-dioxane were stirred for about 4 hours under heating and refluxing and then cooled to room temperature, and the solvent was distilled off under reduced pressure. The concentrated residue was purified by silica gel column chromatography to obtain 370 mg of N-methyl-1-(2-methyl-2-(3-chloro-5-trifluoromethyl-2-pyridyl)hydrazino)-2-nitroetheneamine (Compound No. 35) having a melting point of from 159 to 160° C. (decomposed).

Aufarbeitung

  1. temperatureunder heating
  2. temperaturerefluxing
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe concentrated residue was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-6746119f033842d3b84ae240032f3406
Quelldatensatz
uspto-grants-2002_09
Patentnummer
US06451792B1

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