関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Aminopyridine | HCID 1727 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Pivaloyl chloride | HCID 62493 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(2,2,2-Trimethylacetamido)pyridine | HCID 427059 | 87% |
反応手順
4-Aminopyridine (4.70 g) and triethylamine (6.31 g) were dissolved in dichloromethane (75 ml) to prepare a solution which was then cooled to 0° C. A solution of pivaloyl chloride (6.63 g) in dichloromethane (10 ml) was gradually added dropwise thereto, and the mixture was stirred at 0° C. for 15 min. Thereafter, the reaction solution was stirred at room temperature overnight. The reaction solution was poured into water (50 ml). The dichloromethane layer was washed with a dilute aqueous sodium hydrogencarbonate solution and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by column chromatography using chloroform to give 2,2-dimethyl-N-pyridin-4-yl-propionamide (7.70 g, yield 87%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07560558B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-33d579f4efb9499e88804f033d85b257 |
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| 出典メモ | uspto-grants-2009_07 |
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