1,3,5-Tri-tert-butylbenzene → bis (1,3,5-tri(tertbutyl)benzene) Yttrium

HRID 1074127

Reaktionsgleichung

Reaktionsgleichung von HRID 1074127
[Y:1].[C:2]([C:6]1[CH:11]=[C:10]([C:12]([CH3:15])([CH3:14])[CH3:13])[CH:9]=[C:8]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:7]=1)([CH3:5])([CH3:4])[CH3:3]>>[Y:1].[C:2]([C:6]1[CH:7]=[C:8]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:9]=[C:10]([C:12]([CH3:15])([CH3:14])[CH3:13])[CH:11]=1)([CH3:5])([CH3:4])[CH3:3].[C:2]([C:6]1[CH:7]=[C:8]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:9]=[C:10]([C:12]([CH3:15])([CH3:14])[CH3:13])[CH:11]=1)([CH3:5])([CH3:4])[CH3:3]

Komponenten

3

Edukt 2

HCID 150891,3,5-Tri-tert-butylbenzeneHCID 23993Yttrium

Produkt 1

HCID 86744356bis (1,3,5-tri(tertbutyl)benzene) Yttrium

Versuchsvorschrift

Vapourised yttrium [ca 0.9 g (10 mmol)] was cocondensed with 25 g (100 mmol) of 1,3,5-tri(tertbutyl) benzene at -196° C. over a period of 2 hours. The cocondensate was allowed to warm to room temperature under argon and the solid products extracted from the apparatus with n-hexane (ca 750 cm3). The resultant deep purple solution was filtered through a bed of Celite on a frit and the solvent removed under reduced pressure. Excess of the 1,3,5-tri(tertbutyl)benzene was then removed by the sublimation at 60° C./10-4 mbar and the residue extracted with n-pentane (ca 150 cm3). The resulting solution was again filtered through Celite. Concentration of the resultant solution under reduced pressure and cooling to -30° C. afforded deep purple crystals of the complex. The crystals were collected, washed with n-pentane at -80° C. (2×10 cm3) and dried in vacuo. Yield ca 2.4 g (40% based on yttrium).

Aufarbeitung

  1. extractionthe solid products extracted from the apparatus with n-hexane (ca 750 cm3)
  2. filtrationThe resultant deep purple solution was filtered through a bed of Celite on a frit
  3. customthe solvent removed under reduced pressure
  4. customExcess of the 1,3,5-tri(tertbutyl)benzene was then removed by the sublimation at 60° C./10-4 mbar
  5. extractionthe residue extracted with n-pentane (ca 150 cm3)
  6. filtrationThe resulting solution was again filtered through Celite
  7. temperatureConcentration of the resultant solution under reduced pressure and cooling to -30° C.
  8. customafforded deep purple crystals of the complex
  9. customThe crystals were collected
  10. washwashed with n-pentane at -80° C. (2×10 cm3)
  11. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-17e7c40d34d64869b0bba607f20e1c6e
Quelldatensatz
uspto-grants-1990_11
Patentnummer
US04973498

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