Reaktion #76552

ord-0b634928acbd479e840b5918ccb762cd

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was heated on a steam bath for 30 minutes
  2. 2
    Filtrationfiltered
  3. 3
    WaschenThe filtrate was washed with bicarbonate
  4. 4
    Einengenconcentrated under vacuum
  5. 5
    SonstigeThe residue was recrystallized from isopropanol

Vorschrift

Triethylamine (11.46 mL) was added to a suspension of 3-amino-6-methylquinolin-4-ol hydrochloride in dichloromethane (400 mL). Butyryl chloride (4.46 mL) was added. The reaction mixture was heated on a steam bath for 30 minutes. The solution was diluted with sodium bicarbonate and then filtered. The filtrate was washed with bicarbonate and then concentrated under vacuum. The residue was recrystallized from isopropanol to provide 3-butyramido-6-methylquinolin-4-ol hemihydrate as a solid, m.p. 274-277° C. Analysis: Calculated for C14H16N2O2.½ H2O: %C, 66.39; %H, 6.76; %N, 11.06; Found: %C, 66.56; %H, 6.46; %N, 11.03.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06703402B2uspto-grants-2004_03