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

Hydrochloric Acid → HCID 14012549, Verbindung

HRID 568611
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 568611
[Cl-].[Al+3].[Cl-].[Cl-].[F:5][C:6]1[CH:14]=[CH:13][CH:12]=[CH:11][C:7]=1[C:8](Cl)=[O:9].[Cl:15][C:16]1[C:26]([Cl:27])=[CH:25][CH:24]=[CH:23][C:17]=1[O:18][CH2:19][C:20]([OH:22])=[O:21].Cl>C(=S)=S>[Cl:15][C:16]1[C:26]([Cl:27])=[C:25]([C:8](=[O:9])[C:7]2[CH:11]=[CH:12][CH:13]=[CH:14][C:6]=2[F:5])[CH:24]=[CH:23][C:17]=1[O:18][CH2:19][C:20]([OH:22])=[O:21]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 98082-Fluorobenzoyl chlorideHCID 181052,3-Dichlorophenoxyacetic acidHCID 6451240Aluminum(III) Chloride

Produkt 1

HCID 14012549HCID 14012549, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6348
Carbon Disulfide
Lösungsmittel

Versuchsvorschrift

To a mixture of 12.5 g of aluminum chloride and 45 ml of carbon disulfide there is added dropwise 7.1 g of 2-fluorobenzoyl chloride while maintaining the temperature below 0° C. This low temperature is maintained for 1.5 hours. While maintaining this same low temperature, 5 g of 2,3-dichlorophenoxyacetic acid is added incrementally. After addition is complete, the reaction mixture is maintained at this low temperature for 30 minutes and then permitted to reach ambient temperature after which it is refluxed for 28 hours. The carbon disulfide is decanted from the refluxed solution leaving dark orange residue which is poured onto a mixture of 500 ml of ice/water and 100 ml of concentrated hydrochloric acid. The resulting pink precipitate is collected by filtration, rinsed with 300 ml of warm water (50° C.) and dried in vacuum oven. The dried product is recrystallized twice from aqueous ethyl alcohol to form the product 2,3-dichloro-4-(2-fluorobenzoyl)phenoxyacetic acid having a melting point of 153° to 156° C.

Aufarbeitung

  1. temperaturewhile maintaining the temperature below 0° C
  2. temperatureThis low temperature is maintained for 1.5 hours
  3. additionis added incrementally
  4. additionAfter addition
  5. temperaturethe reaction mixture is maintained at this low temperature for 30 minutes
  6. customto reach ambient temperature
  7. temperatureis refluxed for 28 hours
  8. customThe carbon disulfide is decanted from the refluxed solution
  9. customleaving dark orange residue which
  10. filtrationThe resulting pink precipitate is collected by filtration
  11. washrinsed with 300 ml of warm water (50° C.)
  12. customdried in vacuum oven
  13. customThe dried product is recrystallized twice from aqueous ethyl alcohol

Quellen und Nachweise

ORD-Eintrag
ord-faf0d308b82741f4b56eaa7823104b72
Quelldatensatz
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04728662

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion