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4-Chloro-2-methyl-1H-indene → 4-(3',5'-Di-t-butylphenyl)-2-methylindene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Chloro-2-methyl-1H-indene | HCID 12010742 | — |
| 反応物 | HCID 178441125 | HCID 178441125 | — |
| 触媒 | HCID 178418751 | HCID 178418751 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 4-(3',5'-Di-t-butylphenyl)-2-methylindene | HCID 12010743 | — |
反応手順
4-Chloro-2-methylindene (6.1 g, 37 mmol) and NiCl2(PPh3)2 (1.8 g, 2.8 mmol) were dissolved in 150 mL of Et2O. 3,5-Di-t-butylphenylmagnesium bromide (10 g, 37 mmol) as a Et2O solution was added to the solution and the reaction was stirred overnight at room temperature. After overnight stirring, the reaction was slowly quenched with H2O to neutralize unreacted Grignard. The solution was subsequently treated with 100 mL of 10% HCl(aq), neutralized with saturated sodium bicarbonate aqueous solution. The organic layer was dried with magnesium sulfate and the solvent was removed by rotary evaporation. The remaining residue was loaded onto a silica gel column and eluted with hexane. Yield was 4.6 g (40%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06376413B1 |
| 出典データセット | uspto-grants-2002_04 |
| ORD ID | ord-17559658361f4829b51259a145a097a0 |
| 出典メモ | uspto-grants-2002_04 |