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

Hydrochloric Acid → 3,6-Dichloro-5-trifluoromethyl-2-pyridone

HRID 464131
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 464131
[OH-:1].[K+].[Cl:3][C:4]1[C:9]([Cl:10])=[CH:8][C:7]([C:11]([F:14])([F:13])[F:12])=[C:6]([Cl:15])[N:5]=1.Cl>C(O)(C)(C)C>[Cl:10][C:9]1[C:4](=[O:1])[NH:5][C:6]([Cl:15])=[C:7]([C:11]([F:14])([F:13])[F:12])[CH:8]=1.[Cl:10][C:9]1[CH:8]=[C:7]([C:11]([F:14])([F:13])[F:12])[C:6](=[O:1])[NH:5][C:4]=1[Cl:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 27606902,3,6-Trichloro-5-(trifluoromethyl)pyridine

Produkt 2

HCID 134917763,6-Dichloro-5-trifluoromethyl-2-pyridoneHCID 134917775,6-Dichloro-3-trifluoromethyl-2-pyridone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6386
tert-Butanol
Lösungsmittel

Versuchsvorschrift

To a solution of 2.7 g of potassium hydroxide dissolved in 37 ml of t-butanol was added 6.0 g of 2,3,6-trichloro-5-trifluoromethylpyridine, and the solution was reacted at 80° C. for 3 hours while stirring. After completion of the reaction, the reaction product was allowed to cool and made acidic with concentrated hydrochloric acid. The solvent was distilled off under reduced pressure, and the residue was extracted with methylene chloride. The methylene chloride solution was washed with water and dried over anhydrous sodium sulfate. The methylene chloride was distilled off under reduced pressure, and the resulting residue was passed through a silica gel column (eluent: an n-hexane-ethyl acetate (3:1 by weight) mixture) to obtain 1.5 g of 3,6-dichloro-5-trifluoromethyl-2-pyridone having a melting point of 129° to 131° C. and 0.8 g of 5,6-dichloro-3-trifluoromethyl-2-pyridone having a melting point of 163° to 165° C., respectively.

Aufarbeitung

  1. customthe solution was reacted at 80° C. for 3 hours
  2. customAfter completion of the reaction
  3. temperatureto cool
  4. distillationThe solvent was distilled off under reduced pressure
  5. extractionthe residue was extracted with methylene chloride
  6. washThe methylene chloride solution was washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. distillationThe methylene chloride was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-c73373fb0e594425b6e2b10ff428bd3d
Quelldatensatz
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04546191

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion