関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4,7-dimethyl-1H-indene | HCID 81458 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 178506817 | HCID 178506817 | — |
反応手順
38.2 g (265 mmol) of 4,7-dimethylindene were dissolved in 350 ml of tetrahydrofuran, and the temperature of the solution was taken to 0° C. 165 ml of n-butyllithium (1.6 M in hexane, 264 mmol) were then added dropwise drop over 2.5 hours. After returning to room temperature and continued stirring for 4 hours, a red-purple solution of 4,7-dimethylindenyllithium was obtained. This solution was cooled to −70° C. and treated dropwise in the course of 35 minutes with 25.3 g of 1,2-dibromoethane (135 mmol) in 15 ml of tetrahydrofuran. After returning to room temperature, this gave a clear yellow solution, to which water was added. The organic phase was collected and dried over Na2SO4. The solvent was then evaporated in vacuum, 20 g of product (48% yield) being obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06664351B1 |
|---|
| 出典データセット | uspto-grants-2003_12 |
|---|
| ORD ID | ord-396ba1990a0c4a85be2e6babd6230814 |
|---|
| 出典メモ | uspto-grants-2003_12 |
|---|