Hydrazine hydrate (1:1) → HCID 178526552, Verbindung

HRID 385742Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 385742
C[N:2](/[CH:4]=[N:5]/[C:6]([C:8]1[S:9][C:10]([N+:13]([O-:15])=[O:14])=[CH:11][CH:12]=1)=O)C.O.[NH2:17]N>CC(O)=O>[N+:13]([C:10]1[S:9][C:8]([C:6]2[N:5]=[CH:4][NH:2][N:17]=2)=[CH:12][CH:11]=1)([O-:15])=[O:14]

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 178484334HCID 178484334, Verbindung

Produkt 1

HCID 178526552HCID 178526552, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

N-[(1E)-(Dimethylamino)methylene]-5-nitrothiophene-2-carboxamide (7.00 g, 30.8 mmol) was combined with AcOH (70 mL) and hydrazine hydrate (65% wt, 2.76 mL, 37.0 mmol) and stirred at 90° C. for 1.5 h. The yellow solution was cooled to room temperature and concentrated. The resulting slurry was diluted with CH2Cl2 and saturated NaHCO3 and stirred. The yellow precipitate was isolated by filtration and dried to provide the title compound as a yellow solid.

Aufarbeitung

  1. temperatureThe yellow solution was cooled to room temperature
  2. concentrationconcentrated
  3. additionThe resulting slurry was diluted with CH2Cl2 and saturated NaHCO3
  4. stirringstirred
  5. customThe yellow precipitate was isolated by filtration
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-b36b9329cb3545db8ca49daa2f1197f4
Quelldatensatz
uspto-grants-2013_02
Patentnummer
US08367706B2

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