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Bis(4-bromo-2-methyl-1h-inden-1-yl)dimethylsilane → bis[4-(3-trifluoromethylphenyl)-2-methyl-1H-inden-1-yl](dimethyl)silane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bis(4-bromo-2-methyl-1h-inden-1-yl)dimethylsilane | HCID 59832509 | — |
| 反応物 | HCID 178506173 | HCID 178506173 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 触媒 | HCID 178418851 | HCID 178418851 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | bis[4-(3-trifluoromethylphenyl)-2-methyl-1H-inden-1-yl](dimethyl)silane | HCID 58897762 | — |
反応手順
In an argon atmosphere, to a solution of 28.0 ml of 15 mL of THF with 0.5 M ZnCl2 (14.0 mmol) in THF, 12.3 ml of 1.02 M 3-trifluoromethylphenylmagnesium bromide (12.6 mmol) in THF was added at ambient temperature. This mixture was stirred for 1 hour, and, then, 9.66 ml of 0.02 M Pd(PtBu3)2 (0.19 mmol, 4 mol. %) in THF and 2.42 g (4.83 mmol) of 1 were added. The resulting mixture was stirred for 5 hours at reflux. The product was isolated by flash chromatography on Silica Gel 60 (40-63 μm, d 30 mm, l 100 mm; eluent: hexanes). Yield 2.86 g (98%) of white solid of ca. 1 to 1 mixture of rac- and meso-compounds.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07910783B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-69344f60c9a84019951f7a27eaf00ce5 |
| 出典メモ | uspto-grants-2011_03 |