Allyl Alcohol → HCID 20482369, Verbindung

HRID 648183Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 648183
[H-].[Na+].[CH2:3]([OH:6])[CH:4]=[CH2:5].[H][H].Br[C:10]1[S:11][C:12]([C:15](=[O:19])[N:16]([CH3:18])[CH3:17])=[CH:13][N:14]=1>CN(C)C=O.O>[CH2:3]([O:6][C:10]1[S:11][C:12]([C:15](=[O:19])[N:16]([CH3:18])[CH3:17])=[CH:13][N:14]=1)[CH:4]=[CH2:5]

Komponenten

7

Edukt 4

HCID 7858Allyl AlcoholHCID 24758Sodium hydrideHCID 204823682-bromo-N,N-dimethyl-1,3-thiazole-5-carboxamideHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 20482369HCID 20482369, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a stirred suspension of 0.5 g (10 mmol) of sodium hydride in 5 ml of dry N,N-di-methylformamide under N2, there can be added 0.6 g (10 mmol) of sieve-dried allyl alcohol. After hydrogen evolution ceases, the stirred solution can be treated with 2-bromo-5-(N,N-dimethylcarbamoyl)thiazole (2.35 g, 10.0 mmole). The mixture can then be stirred at 40° under N2 for 18 hours, diluted with four volumes of water and extracted with ether. The ether extracts can be washed with water, dried (Na2SO4), filtered and concentrated in vacuo to give an oil which can then be distilled to give pure title compound.

Aufarbeitung

  1. extractionextracted with ether
  2. washThe ether extracts can be washed with water
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customto give an oil which
  7. distillationcan then be distilled

Quellen und Nachweise

ORD-Eintrag
ord-fe7237d345e04ac1b1577aef2ef9156c
Quelldatensatz
uspto-grants-1983_10
Patentnummer
US04411899

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