StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Thioacetamide → Ethyl 2-(2-methylthiazol-5-yl)acetate

HRID 972834
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 972834
Br[CH:2]([CH:9]=O)[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[C:11]([NH2:14])(=[S:13])[CH3:12]>ClC(Cl)C>[CH3:12][C:11]1[S:13][C:2]([CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5])=[CH:9][N:14]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 2723949ThioacetamideHCID 15576269Ethyl 3-bromo-4-oxobutanoate

Produkt 1

HCID 20388951Ethyl 2-(2-methylthiazol-5-yl)acetateAusbeute 32,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 63651,1-DichloroethaneLösungsmittel2×

Versuchsvorschrift

A mixture of 28.7 g of ethyl 3-bromo-4-oxo-butyrate, 300 ml of dichloroethane and 11.2 g of thioacetamide was refluxed for 10 hours with stirring while replacing the dichloroethane that distilled to keep the volume constant and then the mixture was cooled to room temperature. The mixture was evaporated to dryness and the residue was dissolved in ethyl acetate. The solution was extracted with 2N hydrochloric acid and the pH of the aqueous extracts was made alkaline by addition of ammonium hydroxide. The mixture was extracted with ethyl acetate and the organic extract was washed with water, dried and evaporated to dryness to obtain 8.3 g of ethyl 2-methyl-5-thiazole acetate. The IR spectrum in CHCl3 showed ester C=O at 1737cm-1 and C=C and C=N at 1535cm-1.

Aufarbeitung

  1. temperaturewas refluxed for 10 hours
  2. distillationthat distilled
  3. customThe mixture was evaporated to dryness
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. extractionThe solution was extracted with 2N hydrochloric acid
  6. additionby addition of ammonium hydroxide
  7. extractionThe mixture was extracted with ethyl acetate
  8. extractionthe organic extract
  9. washwas washed with water
  10. customdried
  11. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-2019cab32ea346b89823cb91605b7429
Quelldatensatz
uspto-grants-1977_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04053618

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion