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Dicyclohexylcarbodiimide → HCID 178512296, Verbindung

HRID 864486
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 864486
[C:1]([NH:3][C:4]([NH:6][C:7]1[CH:12]=[CH:11][N:10]=[CH:9][CH:8]=1)=S)#[N:2].[C:13]1([NH:19][CH2:20][CH2:21][NH2:22])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C1(N=C=NC2CCCCC2)CCCCC1>CN(C)C=O>[C:1]([NH:3][C:4]([NH:22][CH2:21][CH2:20][NH:19][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[N:6][C:7]1[CH:12]=[CH:11][N:10]=[CH:9][CH:8]=1)#[N:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 10868DicyclohexylcarbodiimideHCID 742701,2-Ethanediamine, N1-phenyl-HCID 13358277N-Cyano-N'-pyridin-4-ylthiourea

Produkt 1

HCID 178512296HCID 178512296, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

N-Cyano-N'-4-pyridylthiourea (1.80 g) was suspended in dimethylformamide (5 ml). While stirring in an ice bath N-phenylethylenediamine (1.4 ml) and N,N'-dicyclohexylcarbodiimide (2.50 g) were added, resulting in a clear solution. The mixture was left at room temperature for 3 days, when the suspension formed was evaporated extensively under high vacuum. The residue was triturated repeatedly with ether (15 ml portions), and the residual solid was extracted with 1N hydrochloric acid (50 ml). After filtration, the crude product was precipitated from the filtrate by addition of 9N sodium hydroxide and taken up into ethyl acetate (3×75 ml).

Aufarbeitung

  1. additionwere added
  2. customresulting in a clear solution
  3. customwhen the suspension formed
  4. customwas evaporated extensively under high vacuum
  5. customThe residue was triturated repeatedly with ether (15 ml portions)
  6. extractionthe residual solid was extracted with 1N hydrochloric acid (50 ml)
  7. filtrationAfter filtration
  8. customthe crude product was precipitated from the filtrate by addition of 9N sodium hydroxide

Quellen und Nachweise

ORD-Eintrag
ord-2f5c64496bf24f46bd86a4b03a980dc2
Quelldatensatz
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05563160

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