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2-Aminothiazole → HCID 178522552, Verbindung

HRID 1155060
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1155060
[NH2:1][C:2]1[S:3][CH:4]=[CH:5][N:6]=1.[F:7][C:8]([F:24])([F:23])[C:9]1[C:18]([C:19](Cl)=[O:20])=[C:17]([OH:22])[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[N:10]=1>N1C=CC=CC=1>[F:24][C:8]([F:7])([F:23])[C:9]1[C:18]([C:19]([NH:1][C:2]2[S:3][CH:4]=[CH:5][N:6]=2)=[O:20])=[C:17]([OH:22])[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[N:10]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 21552-AminothiazoleHCID 1785211152-Trifluoromethyl-4-hydroxy-3-quinoline-carboxylic acid chloride

Produkt 1

HCID 178522552HCID 178522552, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel2×

Versuchsvorschrift

7.5 g of 2-amino-thiazole and 20 ml of pyridine were added to a solution of the product of Step F in 120 ml of anhydrous pyridine and the mixture was heated at 80°-85° C. for one hour. The mixture was stirred at room temperature for 16 hours and was then evaporated to dryness. The residue was triturated with 200 ml of water and was then vacuum filtered. The filter was washed and the combined wash water and filtrate were cooled in ice and acidified with concentrated hydrochloric acid. The mixture was vacuum filtered and the recovered product was washed with water and dried to obtain 13.7 g of 2-trifluoromethyl-4-hydroxy-N-(2-thiazolyl)-3-quinoline-carboxamide melting at >280° C.

Aufarbeitung

  1. temperaturethe mixture was heated at 80°-85° C. for one hour
  2. customwas then evaporated to dryness
  3. customThe residue was triturated with 200 ml of water
  4. filtrationvacuum filtered
  5. washThe filter was washed
  6. washthe combined wash water and filtrate
  7. temperaturewere cooled in ice
  8. filtrationfiltered
  9. washthe recovered product was washed with water
  10. customdried

Quellen und Nachweise

ORD-Eintrag
ord-271c20c7c2eb40fc89d5a96d3541c65e
Quelldatensatz
uspto-grants-1981_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04299831

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