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Acetic Acid → HCID 21325993, Verbindung

HRID 1701350
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1701350
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]([C:6]([C:8]2[CH:9]=[C:10](CC#N)[CH:11]=[CH:12][CH:13]=2)=[O:7])=[CH:4][CH:3]=1.O.S(=O)(=O)(O)O.[C:25]([OH:28])(=[O:27])[CH3:26]>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([C:8]2[CH:13]=[C:12]([CH2:26][C:25]([OH:28])=[O:27])[CH:11]=[CH:10][CH:9]=2)=[O:7])=[CH:17][CH:18]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 4

HCID 176Acetic AcidHCID 962WaterHCID 1118Sulfuric AcidHCID 53835796HCID 53835796, Verbindung

Produkt 1

HCID 21325993HCID 21325993, Verbindung

Versuchsvorschrift

A mixture of 9.61 g of 3-p-chlorobenzoyl phenyl acetonitrile, 75 cc of water, 75 cc of acetic acid and 75 cc of sulfuric acid was refluxed with stirring for 21/2 hours and then cooled and iced for 1 hour. The mixture was vacuum filtered and the precipitate was empasted with water and taken up in 50 cc of a 10% aqueous sodium carbonate solution. The solution was filtered and the filter was washed with water. The pH of the filtrate was adjusted to 5-6 by addition of acetic acid and after being iced for 30 minutes, the mixture was vacuum filtered. The recovered precipitate was washed with water and dried under reduced pressure. The residue was dissolved in 50 cc of refluxing toluene and the solution was treated with activated carbon and filtered. The filter was washed with boiling toluene. The filtrate was cooled and iced for 1 hour and then vacuum filtered. The recovered precipitate was empasted with iced toluene and dried under reduced pressure to obtain 8.37 g of 3-p-chlorobenzoyl phenyl-acetic acid melting at 148° C.

Aufarbeitung

  1. temperaturewas refluxed
  2. temperaturecooled
  3. waiticed for 1 hour
  4. filtrationfiltered
  5. filtrationThe solution was filtered
  6. washthe filter was washed with water
  7. additionThe pH of the filtrate was adjusted to 5-6 by addition of acetic acid
  8. waitafter being iced for 30 minutes
  9. filtrationfiltered
  10. washThe recovered precipitate was washed with water
  11. customdried under reduced pressure
  12. dissolutionThe residue was dissolved in 50 cc of refluxing toluene
  13. additionthe solution was treated with activated carbon
  14. filtrationfiltered
  15. washThe filter was washed with boiling toluene
  16. temperatureThe filtrate was cooled
  17. waiticed for 1 hour
  18. filtrationvacuum filtered
  19. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-55ec496af97449e596e7c19d7617e700
Quelldatensatz
uspto-grants-1980_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04192890

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