関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 2-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)ethan-1-one | HCID 21984867 | — |
| 反応物 | HCID 178418287 | HCID 178418287 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 1-(4-Chlorophenyl)-2-(2,4-dichlorophenyl)ethane-1,2-dione | HCID 22066077 | — |
反応手順
2-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)ethanone (2.7 g, 9.01 mmol) was dissolved in 1,2-dichloroethane (25 ml) and freshly made PCC (3.89 g, 18.02 mmol), pyridine (1.43 g, 18.02 mmol) and molecular sieves were added. The reaction mixture was refluxed under inert atmosphere overnight. The solution was cooled to 25° C., filtered through Silica and then solvent was evaporated under reduced pressure. The crude product (1.9 g, 66%) was used directly in the next step. 1H NMR (500 MHz) δ 7.97 (d, 2H), 7.84 (d, 1H), 7.52 (d, 2H), 7.46 (s, 1H), 7.44 (d, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07473693B2 |
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| 出典データセット | uspto-grants-2009_01 |
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| ORD ID | ord-51ee4d950a064eb9828639cacff9be8e |
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| 出典メモ | uspto-grants-2009_01 |
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