Acetyl chloride → Methyl 2-phenyl-1,3-thiazole-5-carboxylate

HRID 2256810Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2256810
[C:1](Cl)(=O)C.[C:5]1([C:11]2[S:12][C:13]([C:16]([OH:18])=[O:17])=[CH:14][N:15]=2)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1>CO>[C:5]1([C:11]2[S:12][C:13]([C:16]([O:18][CH3:1])=[O:17])=[CH:14][N:15]=2)[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1

Komponenten

4

Edukt 2

HCID 6367Acetyl chlorideHCID 1390872-Phenyl-5-carboxythiazole

Produkt 1

HCID 18913489Methyl 2-phenyl-1,3-thiazole-5-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

2.5 ml of acetyl chloride were added to a solution of 4.77 g of the acid of Stage B in 160 ml of methanol, and the mixture was refluxed for 18 hours. After evaporating to dryness under reduced pressure, the residue was taken up in ethyl acetate. The mixture was filtered and concentrated to a reduced volume. The crystals were separated off and the mother liquors were washed with sodium hydroxide. Extraction was carried out with ethyl acetate, followed by washing with water and evaporating to dryness. The 2 crystallized fractions were combined to obtain 4.54 g of the desired product melting at 108° C.

Aufarbeitung

  1. temperaturethe mixture was refluxed for 18 hours
  2. customAfter evaporating to dryness under reduced pressure
  3. filtrationThe mixture was filtered
  4. concentrationconcentrated to a reduced volume
  5. customThe crystals were separated off
  6. washthe mother liquors were washed with sodium hydroxide
  7. extractionExtraction
  8. washby washing with water
  9. customevaporating to dryness

Quellen und Nachweise

ORD-Eintrag
ord-272f3d0548564e16b3427e213d9500ae
Quelldatensatz
uspto-grants-1997_08
Patentnummer
US05656607

Notizen zur Reaktion

Wird geladen…