関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2-Fluoropyridine | HCID 9746 | — |
| 反応物 | 1,4-Benzenedimethanol | HCID 11506 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (4-(Pyridin-2-yloxymethyl)-phenyl)-methanol | HCID 59255473 | 67.9% |
反応手順
To a mixture of 1,4-benzenedimethanol (5.5 g, 40 mmol), 2-fluoropyridine (1.3 g, 13 mmol) and N,N-dimethylformamide (15 mL) was added sodium hydride (1.4 g, 40 mmol, 66% in oil) at 0° C., which was stirred for 20 minutes at room temperature and for 1 hour at 70° C. Water was added to the reaction mixture, which was then extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, and the solvent was evaporated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=1:1) to obtain the title compound (1.9 g, 66%).
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-76c644397f444352bb4e0c7420741d8f |
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| 出典メモ | uspto-grants-2014_09 |
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