関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,3,5-Tri-tert-butylbenzene | HCID 15089 | — |
| 反応物 | Yttrium | HCID 23993 | — |
| 生成物 | 1,3,5-tri(tertbutyl)benzene Yttrium | HCID 86743687 | — |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04894446 |
|---|
| 出典データセット | uspto-grants-1990_01 |
|---|
| ORD ID | ord-0b241699311f44d8a2914b29b90705cc |
|---|
| 出典メモ | uspto-grants-1990_01 |
|---|