1,3,5-Tri-tert-butylbenzene → 1,3,5-tri(tertbutyl)benzene Yttrium
反応式
[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]参加物
3
実験手順
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).
後処理
- extraction