反应详情

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).

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