Hydrazine → HCID 178489941, Verbindung

HRID 38083

Reaktionsgleichung

Reaktionsgleichung von HRID 38083
[S:1]1CS[C:2]1=[C:5]([C:16]1[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=1)[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH3:15])[CH:9]=1)=O.[NH2:22][NH2:23]>C1COCC1>[CH3:15][O:14][C:10]1[CH:9]=[C:8]([C:6]2[C:5]([C:16]3[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=3)=[C:2]([SH:1])[NH:22][N:23]=2)[CH:13]=[CH:12][CH:11]=1

Komponenten

4

Edukt 2

HCID 9321HydrazineHCID 866585382-[1,3]Dithietan-2-ylidene-1-(3-methoxy-phenyl)-2-pyridin-4-yl-ethanone

Produkt 1

HCID 178489941HCID 178489941, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

2-[1,3]Dithietan-2-ylidene-1-(3-methoxy-phenyl)-2-pyridin-4-yl-ethanone (1.18 g, 3.17 mmol) was suspended into a 1 M solution of hydrazine in THF and heated to 70° C. for two hours. The suspension was then concentrated under reduced pressure, taken up with a small volume of ethanol and diluted with THF (10 mL) and stirred for 5 minutes. The solid was filtered, washed with THF and dried at 50° C. for 2 hours. 1.26 g of 5-(3-methoxy-phenyl)-4-pyridin-4-yl-2H-pyrazole-3-thiol were obtained as an orange solid and used in the following step without further purification.

Aufarbeitung

  1. concentrationThe suspension was then concentrated under reduced pressure
  2. additiondiluted with THF (10 mL)
  3. filtrationThe solid was filtered
  4. washwashed with THF
  5. customdried at 50° C. for 2 hours

Quellen und Nachweise

ORD-Eintrag
ord-45f594149cd64d9aaea3895cce1eff2d
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08524707B2

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