関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Solketal | HCID 7528 | — |
| 反応物 | 2-Amino-4-chloropyridine | HCID 581866 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-((2,2-Dimethyl-1,3-dioxolan-4-yl)methoxy)pyridin-2-amine | HCID 50987595 | 80% |
反応手順
A sealed tube containing 4-chloro-2-pyridinamine (4 g, 31.2 mmol), (2,2-dimethyl-1,3-dioxolan-4-yl)methanol (8.4 g, 60.6 mmol), and sodium (1.46 g, 63.5 mmol) was heated at 145° C. for 8 hours. The mixture was cooled to ambient temperature; water (25 mL) and dichloromethane (50 mL) were added. The organic phase was separated, dried with sodium sulfate, and concentrated under reduced pressure. The resulting residue was purified by chromatography on silica-gel to give 4-((2,2-dimethyl-1,3-dioxolan-4-yl)methoxy)pyridin-2-amine as a pale yellow solid (5.6 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08841455B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-5231720e43f441fda1d0c65964eaca65 |
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| 出典メモ | uspto-grants-2014_09 |
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