Mesitylene → Vanadium bis-mesitylene

HRID 248547

Reaktionsgleichung

Reaktionsgleichung von HRID 248547
[Al].[Al+3].[Cl-].[Cl-].[Cl-].[C:6]1([CH3:14])[CH:11]=[C:10]([CH3:12])[CH:9]=[C:8]([CH3:13])[CH:7]=1.O(Cl)Cl.[V:18]>O1CCCC1.C(COC)OC>[C:6]1([CH3:14])[CH:11]=[C:10]([CH3:12])[CH:9]=[C:8]([CH3:13])[CH:7]=1.[C:6]1([CH3:14])[CH:11]=[C:10]([CH3:12])[CH:9]=[C:8]([CH3:13])[CH:7]=1.[V:18]

Komponenten

6

Edukt 4

HCID 7947MesityleneHCID 5359268AluminumHCID 6451240Aluminum(III) Chloride2×HCID 86746833Chloro hypochlorite;vanadium

Produkt 1

HCID 11077154Vanadium bis-mesityleneAusbeute 35,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 22732251Tetrahydrofuran dimethoxyethaneLösungsmittel

Versuchsvorschrift

The following products are charged in order into a 250 ml glass flask equipped with a thermometer, magnetic stirrer and reflux cooler: 1.888 g (70 mmoles) of active aluminium metal having the characteristics described in Example 1, AlCl3 (5.6 g; 42 mmoles), mesitylene (43 g; 360 mmoles) and VOCl3 (6.1 g; 35 mmoles), with a molar ratio V:Al:AlCl3 equal to 1:2:1.2. A strong hexothermal reaction takes place. After 1 hour of stirring at room temperature, the mixture is heated for 3 hours to 160°-170° C., and a dark reddish-brown suspension is obtained. After cooling to room temperature, 50 ml of a mixture of tetrahydrofuran-dimethoxyethane 18.85 (v/v) are added to this suspension and vigorous stirring is maintained at room temperature for 3 hours. After filtration, the filtrate is dried (0.1 Torr; 50° C.) and the residue is treated with heptane (50 ml). The resulting solution is filtered, concentrated and cooled to -80° C. 3.6 g of vanadium bis-mesitylene are obtained corresponding to a yield of 35%.

Aufarbeitung

  1. additionThe following products are charged in order into a 250 ml glass flask
  2. customequipped with a thermometer, magnetic stirrer
  3. temperaturereflux cooler
  4. customA strong hexothermal reaction
  5. temperaturethe mixture is heated for 3 hours to 160°-170° C.
  6. customa dark reddish-brown suspension is obtained
  7. temperatureAfter cooling to room temperature
  8. stirringvigorous stirring
  9. temperatureis maintained at room temperature for 3 hours
  10. filtrationAfter filtration
  11. customthe filtrate is dried (0.1 Torr; 50° C.)
  12. additionthe residue is treated with heptane (50 ml)
  13. filtrationThe resulting solution is filtered
  14. concentrationconcentrated
  15. temperaturecooled to -80° C

Quellen und Nachweise

ORD-Eintrag
ord-05daca4bc2e74f618c0452ed6e5b5bf4
Quelldatensatz
uspto-grants-1993_05
Patentnummer
US05210244

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