Hydrazine hydrate (1:1) → HCID 178526614, Verbindung

HRID 38071

Reaktionsgleichung

Reaktionsgleichung von HRID 38071
[S:1]1CS[C:2]1=[C:5]([C:17]1[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=1)[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([N+:14]([O-:16])=[O:15])[CH:9]=1)=O.O.[NH2:24][NH2:25]>C(O)C>[N+:14]([C:10]1[CH:9]=[C:8]([C:6]2[C:5]([C:17]3[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=3)=[C:2]([SH:1])[NH:24][N:25]=2)[CH:13]=[CH:12][CH:11]=1)([O-:16])=[O:15]

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 469291812-[1,3]-Dithietan-2-ylidene-1-(3-nitro-phenyl)-2-pyridin-4-yl-ethanone

Produkt 1

HCID 178526614HCID 178526614, VerbindungAusbeute 83,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

2-[1,3]-Dithietan-2-ylidene-1-(3-nitro-phenyl)-2-pyridin-4-yl-ethanone (5.2 g, 15.7 mmol) was suspended in absolute ethanol (60 mL) and heated to 60° C. Hydrazine monohydrate (3.05 mL, 63 mmol, 4 eq) was added dropwise and the mixture was stirred at 60° C. for 2 hours. The suspension was concentrated to about ¼ of the original volume, diluted with THF (30 mL) and stirred for 5 minutes. The solid was filtered, washed with THF and dried at 50° C. for 2 hours. 3.92 g of 5-(3-nitro-phenyl)-4-pyridin-4-yl-2H-pyrazole-3-thiol were obtained as an orange solid (84%).

Aufarbeitung

  1. concentrationThe suspension was concentrated to about ¼ of the original volume
  2. additiondiluted with THF (30 mL)
  3. stirringstirred for 5 minutes
  4. filtrationThe solid was filtered
  5. washwashed with THF
  6. customdried at 50° C. for 2 hours

Quellen und Nachweise

ORD-Eintrag
ord-0b0f4c38ee9046febed8f9c268fedaf8
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08524707B2

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