関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 反応物 | HCID 178443576 | HCID 178443576 | — |
| 触媒 | HCID 178418745 | HCID 178418745 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1,2-Bis(2-ethylhexyl)benzene | HCID 15920117 | 62% |
反応手順
A dry 2 L 3-neck flask with attached reflux condenser and addition funnel, flushed with dry nitrogen, was charged with 1,2-dichlorobenzene (79.4 g, 540 mmol), Ni(dppp)Cl2 (3 g, 6 mmol), and 200 mL of dry Et2O. The addition funnel was charged with 2-ethylhexylmagnesium bromide (3M, 400 mL). The solution was cooled to 5° C. and the Grignard reagent was added dropwise to the reaction. After complete addition, the reaction was stirred at 5° C. for 30 min and then warmed to room temperature (RT). The reaction was then heated to reflux for 12 h. After cooling to RT, the reaction mixture was poured onto an ice/HCl (10%) solution and extracted with MTBE. The organic fractions were dried over anhydrous MgSO4 and then concentrated. The product was purified first by distillation followed by column chromatography with hexanes, and isolated as colorless oil (101 g, 62%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08440785B2 |
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| 出典データセット | uspto-grants-2013_05 |
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| ORD ID | ord-784f089103ee4d7bbc9bafffc6e47c30 |
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| 出典メモ | uspto-grants-2013_05 |
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