関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N,N'-Dimethylethylenediamine | HCID 8070 | — |
| 反応物 | Ethyl 5,6-diphenylpyridine-2-carboxylate | HCID 14789610 | — |
| 反応物 | Trimethylaluminum | HCID 16682925 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-(5,6-Diphenyl-pyridin-2-yl)-ethanone | HCID 59338826 | — |
反応手順
General Procedure O. To a solution of ethyl 5,6-diphenylpyridine-2-carboxylate (Compound 21, 246 mg, 0.81 mmol) in toluene (5 ml) was added N,N′-dimethylethylenediamine (DMEDA, 78.7 mg, 0.89 mmol) and trimethylaluminum (1.2 ml, 2.44 mmol, 2 M in toluene) dropwise under argon at room temperature. After the mixture was refluxed at 112° C. for 2.5 hours, it was quenched with water, and the products were extracted with ethyl acetate. The combined organic layers were washed with brine, and dried over Na2SO4. The filtered solvents were concentrated in vacuo, and the residue was purified by silica gel chromatography (15% ethyl acetate in hexane) to give title compound as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728014B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-a2896fc6ab234e46af24b98823239a8b |
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| 出典メモ | uspto-grants-2010_06 |
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