Sulfuric Acid → 1,3,5-Tri(4-bromophenyl)benzene

HRID 1404816Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1404816
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([Br:10])=[CH:6][CH:5]=1)=O.S(=O)(=O)(O)O.S(OS([O-])(=O)=O)([O-])(=O)=O.[K+].[K+]>C(O)C>[Br:10][C:7]1[CH:8]=[CH:9][C:4]([C:2]2[CH:1]=[C:2]([C:4]3[CH:9]=[CH:8][C:7]([Br:10])=[CH:6][CH:5]=3)[CH:1]=[C:2]([C:4]3[CH:9]=[CH:8][C:7]([Br:10])=[CH:6][CH:5]=3)[CH:1]=2)=[CH:5][CH:6]=1

Komponenten

5

Edukt 3

HCID 1118Sulfuric AcidHCID 7466p-BromoacetophenoneHCID 62681Potassium pyrosulfate

Produkt 1

HCID 2327611,3,5-Tri(4-bromophenyl)benzeneAusbeute 79,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 0.8 kg of 4-bromoacetophenone by Sigma-Aldrich Japan, KK., 40 ml of sulfuric acid and 1.2 kg of potassium disulfate was stirred at 180° C. for 18 hours. After stirring, 3.0 L of ethanol was added to the mixture, which was heated to reflux for 7 hours. It was then allowed to naturally cool to room temperature, producing a precipitate which was filtered out. After adding 3.0 L of water to the filtered precipitate and heating to reflux for 1 hour, the reaction mixture was allowed to naturally cool to room temperature. The reaction mixture was filtered and rinsed with 0.5 L of ethanol. In this manner there was obtained 0.58 kg of 1,3,5-tris(p-bromophenyl)benzene.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureto reflux for 7 hours
  3. customproducing a precipitate which
  4. filtrationwas filtered out
  5. additionAfter adding 3.0 L of water to the filtered precipitate
  6. temperatureheating
  7. temperatureto reflux for 1 hour
  8. temperatureto naturally cool to room temperature
  9. filtrationThe reaction mixture was filtered
  10. washrinsed with 0.5 L of ethanol

Quellen und Nachweise

ORD-Eintrag
ord-d0caeebb93d24cc58630306b00c04790
Quelldatensatz
uspto-grants-2014_12
Patentnummer
US08915989B2

Notizen zur Reaktion

Wird geladen…