関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Hydroxylamine HCl | HCID 21645 | — |
| 反応物 | 5-Benzyloxy-2-cyanomethylpyridine | HCID 22181385 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178510832 | HCID 178510832 | 27.1% |
反応手順
To an ethanol (30 mL) solution of (5-benzyloxy-pyridin-2-yl)-acetonitrile (1.77 g, 7.89 mmol) described in Manufacturing Example 127-1-4 were added hydroxylammonium chloride (848 mg, 11.8 mmol) and potassium carbonate (2.18 g, 15.8 mmol), which was stirred for 11 hours and 20 minutes at 70° C. The mixture was then stirred for another 5 hours and 45 minutes under reflux. Water was added to the reaction mixture at room temperature, which was extracted with ethyl acetate. The organic layer was separated, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate: methanol=10:1) to obtain the title compound (550 mg, 27%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08841327B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-1d333c4d82c24031895fb51fc7caa696 |
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| 出典メモ | uspto-grants-2014_09 |
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