Dimethylformamide dimethyl acetal → HCID 28887991, Verbindung

HRID 1988806Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1988806
[C:1]1([NH:11][C:12](=[S:15])[NH:13][NH2:14])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[CH3:16]OC(OC)N(C)C>O1CCOCC1>[C:1]1([N:11]2[CH:16]=[N:14][NH:13][C:12]2=[S:15])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

Komponenten

4

Edukt 2

HCID 78373Dimethylformamide dimethyl acetalHCID 2760175N-(Naphthalen-1-yl)hydrazinecarbothioamide

Produkt 1

HCID 28887991HCID 28887991, VerbindungAusbeute 100,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of 4-(1-naphthalenyl)-3-thiosemicarbazide (4.01 g, 18.4 mmol) and N,N,-dimethylformamide dimethyl acetal (2.50 mL, 18.8 mmol) in 1,4-dioxane (40 mL) was stirred at room temperature for 16 h. The mixture was concentrated under reduced pressure. The residue was taken in hexane and Et2O and the solution was stirred until a suspension was obtained. The suspension was filtered and the solid was triturated with hexane:Et2O (4:1), then was dried under reduced pressure to give the title compound (4.19 g, 90% yield) as a beige solid.

Aufarbeitung

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customwas obtained
  3. filtrationThe suspension was filtered
  4. customthe solid was triturated with hexane:Et2O (4:1)
  5. customwas dried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-c1ae9541110a4cd5b3bc31d9aa5cfb60
Quelldatensatz
uspto-grants-2010_01
Patentnummer
US07642277B2

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